Desalination 219 (2008) 250–261

Adsorptive removal of basic dye by chemically activated

Parthenium biomass: equilibrium and kinetic modeling
Hem Lataa, V.K. Gargb, R.K. Guptaa*
a
Department of Chemistry, bDepartment of Environmental Science and Engineering,
Guru Jambheshwar University of Science and Technology, Hisar 125001, Haryana, India
Tel. +91 (1662) 263152; Fax: +91 (1662) 276240; email: rkgic@yahoo.com

Received 19 December 2006; Accepted 6 May 2007

Abstract
This paper reports the removal of a basic dye (rhodamine-B) by the activated carbon prepared from Parthenium
biomass by sulphuric acid treatment method (SWC). The effectiveness of the prepared adsorbent has been studied
as a function of agitation time, adsorbent dosage, initial dye concentration and pH. The removal of rhodamine-B by
SWC followed second order kinetic model. The second order model best describes adsorption kinetic data.
Adsorption data were modeled using both Langmuir and Freundlich classical adsorption isotherms. The adsorption
capacity Q0 was 18.52 mg/g at initial pH 7 for the particle size 0.3–1 mm. The equilibrium time is about 60 min for
the studied initial dye concentrations. Maximum dye removal (99.2%) was obtained at pH 7 using an adsorbent dose
of 16.0 g/L for 50 mg/L dye concentration in the aqueous solution. FT-IR spectra of the adsorbents were recorded
to explore the number and position of functional groups available for the binding of dye onto studied adsorbents. The
presence of O-H, C=O and C-O groups was identified in the adsorbent. SEMs of the native and exhausted (SWC)
were recorded to explore the morphology of the adsorbent.

Keywords: Rhodamine-B; Sulphuric acid; Parthenium; Adsorbent; Adsorption equilibrium; pH; FT-IR; Langmuir;
Adsorbent dose; SEM

1. Introduction paper and pulp manufacturing, dyeing of cloth,

Many industrial processes use different
synthetic chemical dyes for various purposes.
Some frequent users of these chemicals include
*Corresponding author.
leather treatment, printing etc. Most of the used
solutions containing such dyes are discharged as
effluents [1]. The discharge of colored wastes
into receiving streams not only affects the aesthe-
tic nature but also interferes with the transmission
of sunlight into streams and therefore reduces

0011-9164/08/$– See front matter © 2008 Published by Elsevier B.V.

doi:10.1016/j.desal.2007.05.018
 H. Lata et al. / Desalination 219 (2008) 250–261
photosynthetic activity [2]. Wastewaters offer
considerable resistance for their biodegradation
due to the presence of these heat and light stable
dyes, thus upsetting aquatic life [3]. Thus,
pollution caused by industrial wastewaters has
become a common problem for many countries
[4].
Several methods have been tested for color
removal from the industrial effluents to decrease
their impact on the environment. These methods
include adsorption onto inorganic or organic
matrices, decolourization by photo-catalysis or
photo-oxidation processes, microbiological de-
composition, chemical oxidation, ozonation and
coagulation [5]. Adsorption is one of the most
effective processes used for the dye removal from
wastewaters.The biggest barrier in the application
of this process by the industries is the high cost of
adsorbents presently available for commercial
use. The cost of adsorption technology appli-
cation can be reduced if the adsorbent is
inexpensive. Consequently, numerous low cost
alternatives have been proposed including sago
waste [6], waste coir pith [7], Parthenium
hysterophorus [8,9], pine sawdust [10], sugarcane
dust [11], rubber wood sawdust [12], bottom ash
and de-oiled soya [13], palm kernel [14], hen
feathers [15], etc.
Rhodamine is a family of related chemical
compounds, fluorone dyes. Examples are Rhoda-
mine B and Rhodamine 6G. They are used as a
dye and as a dye laser gain medium. It is often
used as a tracer within water to determine the rate
and direction of flow and transport. Rhodamine
dyes are generally toxic, and are soluble in water,
methanol, and ethanol. Rhodamine B is also used
in biology as a staining fluorescent dye, some-
times in combination with auramine O, as the
auramine-rhodamine stain to demonstrate acid-
fast organisms, notably Mycobacterium. Rhoda-
mine B has been tested in mice and rats by sub-
cutaneous injection and in inadequate studies by
oral administration. It was carcinogenic in rats
when injected subcutaneously, producing local
251
sarcomas. The intravenous LD50 in rats is
89.5 mg/kg [www.osha-slc.gov/dts/sltc/methods].
In the present study rhodamine-B removal
efficiency of activated carbon prepared from Par-
thenium biomass by the sulphuric acid treatment
method (SWC) has been tested in batch mode.
The effect of process parameters such as pH,
adsorbent dose, contact time and initial concen-
tration was investigated. The kinetics of rhoda-
mine-B adsorption on SWC was analyzed by
fitting various kinetic models. Experimental
equilibrium data were fitted to the Freundlich and
Langmuir equations to determine the best fit
isotherm equation. Error analysis was carried out
to test the adequacy and the accuracy of the
model equation.
2. Experimental
2.1. Preparation of sulphuric acid treated
parthenium carbon (SWC)
Fully grown plants of Parthenium were col-
lected in and around Hisar City (India), cut into
small pieces of 2–3 cm and dried in sunlight. The
dried biomass was mixed with concentrated
sulphuric acid (1:1.5, w/v) and allowed to stand
at 120EC for 24 h in a hot air oven. The car-
bonized material so obtained was washed with
distilled water several times to remove the free
acid and soaked in 1% sodium bicarbonate
solution overnight to remove any residual acid.
This material was then washed with distilled
water and dried at 105EC in a hot air oven for
24 h. It was ground and sieved in the size range
of 0.3–1.0 mm. The material so obtained was
analyzed for various physicochemical charac-
teristics. The general characteristics of SWC
were: bulk density = 0.57 g/mL, particle size =
0.3–1.0 mm; water solubility (%) = 2.86; acid
solubility (%) = 4.0; moisture content (%) = 0.15;
pH = 7.2; C (%) = 49.40; H (%) = 3.71; N (%) =
2.31; O (%) by difference = 44.58. The presence
of carboxylic and phenolic groups was confirmed
252 H. Lata et al. / Desalination 219 (2008) 250–261
by chemical tests. The material was placed in
airtight plastic containers for further use.
2.2. Adsorbate
The adsorbate, rhodamine-B dye (CI = 45170;
purity = 80%, chemical formula = C28H31ClN2O3;
CAS No. = 81-88-9; FW = 479.02; class = basic
dye; synonyms = rhodamine 610, basic violet 10,
color = bright reddish violet; melting point =
165EC, pH = 7.03 and λmax = 552 nm) was used as
supplied by S.D. Fine Chemical (Mumbai, India).
An accurately weighed quantity of the dye was
dissolved in double distilled water to prepare the
stock solution (1000 mg/l). The percentage purity
of the dye was taken into consideration while
preparing the stock solutions. Experimental
solutions of desired concentration were obtained
by successive dilution.
2.3. Batch mode experiments
To study the effect of process parameters, i.e.,
pH, adsorbent dose, contact time, initial dye
concentration on the adsorptive removal of
rhodamine-B, batch experiments were conducted
at 34±1EC. For each experimental run, 50 ml of
rhodamine-B solution of known concentration,
pH and adsorbent was taken in a 0.25 dm3
stoppered conical flask. This mixture was agitated
on a rotary shaker at a constant speed of 180 rpm.
Samples were withdrawn at pre-determined time
intervals, the adsorbent was separated from the
solution by centrifugation and residual dye
concentration was estimated in the supernatant
spectrophotometrically using an Elico spectro-
photometer (Model SL-177). All experiments
were carried out at pH 7 unless otherwise men-
tioned. Effect of pH on dye removal was studied
over a pH range of 3–10. pH was adjusted by the
addition of dilute (0.01M) aqueous solution HCl
or NaOH. For the optimization of adsorbent dose,
a 50 ml dye solution was contacted with different
quantities of adsorbent (4.0–20.0 g/L) till equili-
brium was attained and it was found to be 16.0
g/L. Kinetics of adsorption was determined by
ana-lyzing adsorptive uptake of the dye from
aqueous solution at different time intervals. The
amount of dye adsorbed onto the adsorbent at
equilibrium, qe (mg/g), was calculated by a mass-
balance relationship:
( C0 − Ce )
qe = V (1)
W
where C0 and Ce are the initial and equilibrium
state dye concentration (mg/l), V is the volume of
solution (l) and W is the mass of adsorbent (g).
The amount of adsorption at time t, qt (mg/g), was
calculated by:
( C0 − Ct )
qt = V (2)
W
where C0 and Ct (mg/g) are the liquid phase con-
centrations of dye at initial and any time t,
respectively. V is the volume of solution (l) and
W is the mass of dry adsorbent (g). For adsorption
isotherms, dye solutions of different concen-
trations were agitated with known amount of
adsorbent till the equilibrium was achieved. The
residual dye concentration was determined as
reported earlier. Blank runs, with only the
adsorbents in 50 ml of double distilled water,
were conducted simultaneously at similar condi-
tions to account for any color leached by the
adsorbents and adsorbed by glass containers.
2.4. Fourier transform infrared analysis (FTIR)
Infrared spectra of the adsorbents was
obtained using a Fourier transform infrared
spectrometer (Perkins-Elmer, PE-RXI). For the
FTIR study, 2 mg of finely ground adsorbent was
encapsulated in 40 mg of KBr in order to prepare
translucent sample disks. From these FT-IR
 H. Lata et al. / Desalination 219 (2008) 250–261 253

spectra, the presence of functional groups in the

adsorbent was confirmed.
The surface morphology of the adsorbents was
analysed by scanning electron microscopy using
a Leo 435 VP scanning electron microscope.

3. Results and discussion

3.1. Effect of pH
Fig. 1. Effect of pH on the adsorption of rhodamine-B by
pH is one of the most important process SWC (dye concentration = 50 mg/L, adsorbent dose =
parameters controlling the adsorption. The effect 4.0 g/L, contact time = 2 h).
of pH on the removal of rhodamine-B is shown in
Fig. 1. The experiments were carried out at
50 mg/L initial dye concentration with a 4.0 g/L
adsorbent dose at 34±1EC temperature for
120 min contact time. The dye adsorption by
SWC was 62.6 to 70.6% in the studied pH range
of 3–10. The percent removal of rhodamine-B
was almost unaffected when the pH was in-
creased from 3–10. Therefore, neutral pH has
been chosen for the further experiments. Similar
behaviour has been reported during the adsorp-
tion of rhodamine-B by biogas waste slurry [16]
and waste banana pith [17].

3.2. Effect of initial dye concentration and

agitation time
The influence of initial dye concentration in
the solution on the rate of adsorption on SWC
was studied. The experiments were carried out at
fixed adsorbent dose (4.0 g/L) in the test solu-
tionat 34±1EC temperature, neutral pH and at
different initial concentrations of rhodamine-B
(50, 100, 150, 200, 250 mg/L) for different time
intervals upto 120 min for attaining equilibrium.
The adsorption of rhodamine-B vs. contact time
at different concentrations is given in (Fig. 2).
The results indicate that the actual amount of dye
adsorbed per unit mass of adsorbent increased
with an increase in rhodamine-B concentration.
This is due to increase in driving force of the
concentration gradient, as an increase in the ini-
Fig. 2. Effect of initial dye concentration on adsorption of
rhodamine-B (adsorbent dose = 4.0 g/L, pH = neutral).
tial dye concentrations. The adsorption capacity
for rhodamine-B at equilibrium increased from
(5.98, 7.31, 10.28 and 10.80) mg/g respectively
as the rhodamine-B concentration increased from
(50, 100, 150, and 250 mg/l). It is also evident
from Fig. 2 that the contact time needed for
rhodamine-B solutions with initial concentrations
of 50–250 mg/l to reach the equilibrium was
about 60 min after that the concentration of
rhodamine-B in liquid phase remained almost
254 H. Lata et al. / Desalination 219 (2008) 250–261
Fig. 3. Effect of adsorbent dose on adsorption of
rhodamine-B (dye concentration = 50 mg/L, volume of
sample = 50 mL, pH = neutral).
constant. The initial portion of curves is linear
and then change into a plateau at levels of 45 and
60 min of contact time. The plateau portion of the
curve corresponds to pore diffusion and linear
portion of curve reflects surface layer diffusion
[18].
3.3. Effect of adsorbent dose
The percent adsorption of rhodamine-B on
SWC was studied at different adsorbent doses
(4.0, 8.0, 12.0, 16.0 and 20 g/L, respectively)
keeping rhodamine-B concentration (50 mg/l),
pH (7.0) and temperature (34±1EC) constant at
different agitation times (15, 30, 45, 60, 90 and
120 min). It is evident from Fig. 3 that dye
adsorption increases in an adsorbent dose. The
percent adsorption increased from 56.5 to 98.7%
at equilibrium as the SWC dose was increased 4.0
to 20 g/L. This was attributed to an increase in
the carbon concentration, which increased the
available surface area and adsorption sites [19].
But adsorption capacity was decreased with an
increase in adsorbent dosage. As the adsorbent
dose was increased from 4.0 to 20 g/L, the
adsorption capacity for SWC decreased from 7.10
Table 1
Some fundamental frequencies of the studied adsorbent
(before and after use)
Band position SWC native SWC-RB
(cm!1)
O-H 3385.9 3448.1
C=O 1708.5 1891.2
C-O 1037.4 1083.4
Bending vibrations 782.4, 611.9 987.3, 957.2, 764.7
to 2.46 mg/g. This may be due to overlapping of
adsorption sites as a result of overcrowding of
adsorbent particles [20].
3.4. Infrared spectroscopy analysis
The FT-IR spectra of SWC before and after
adsorption of rhodamine-B were used to deter-
mine the frequency changes in the functional
groups in the adsorbent. The spectra of adsorbent
were measured within the range of 500–
4000 cm!1. The FT-IR spectra of the adsorbent
displays number of absorption peaks, indicating
the complex nature of studied adsorbent. Table 1
presents the fundamental peaks of the adsorbent
before and after use. An absorption peak around
3385.9 cm!1 represented bonded hydroxyl groups.
The peak observed at 1708.5 cm!1 corresponds to
C=O stretching. The peaks around 1614.7 cm!1
corresponds to the C=C stretching and at 1037.4
cm!1 corresponds to C–O band (Fig. 4a). The
–OH, C=O and C–O band absorption peak is
observed to shift to 3448.1, 1891.2 and
1083.4 cm!1 respectively when SWC is loaded
with rhodamine-B (Fig. 4b). It seems that these
functional groups participate in dye binding.
The SEM images of native SWC (Fig. 5a)
show the porosity and surface structure. After dye
adsorption, a significant change is observed in the
structure of this adsorbent (Fig. 5b) The adsor-
bents appear to have a rough surface and pores
containing a new shiny and bulky particles.
 H. Lata et al. / Desalination 219 (2008) 250–261
Fig. 4a. FT-IR spectra of sulphuric acid treated carbon before use.
3.5. Adsorption isotherm
The adsorption isotherm indicates how the
adsorption molecules distribute between the
liquid phase and the solid phase when the adsorp-
tion process reaches an equilibrium state. The
analysis of the isotherm data by fitting them to
different isotherm models is an important step to
find the suitable model that can be used for
design purpose [21]. Adsorption isotherm study
is carried out on two well known isotherms,
Langmuir and Freundlich. Langmuir isotherm
assumes monolayer adsorption onto a surface
containing a finite number of adsorption sites of
uniform strategies of adsorption with no trans-
migration of adsorbate in the plane of surface
[22] while Freundlich isotherm model assumes
heterogeneous surface energies, in which the
255
energy term in the Langmuir equation varies as a
function of the surface coverage. Judging the
correlation coefficients, R2, we can compare the
applicability of the isotherm equation.
3.5.1. Langmuir isotherm
The linear form of Langmuir isotherm model
is given by the following equation:
Ce 1 1
= + Ce (3)
qe Q0 ⋅ b Q0
where Ce is the equilibrium concentration of the
adsorbate (RB) mg/L, qe is the amount of adsor-
bate adsorbed per unit mass of adsorbent (mg/g),
and Q0 and b are Langmuir constants related to
256 H. Lata et al. / Desalination 219 (2008) 250–261

Fig. 4b. FT-IR spectra of sulphuric acid treated carbon after use.

Fig. 5. Scanning electron micrographs (SEM) of (a) native SWC and (b) SWC after dye adsorption.
 H. Lata et al. / Desalination 219 (2008) 250–261 257

Table 2 Table 3
Values of Langmuir and Freudnlich parameters obtained Adsorption capacities of different low-cost adsorbents for
for the studied systems the removal of different dyes from its aqueous solutions

Adsorbent (Rhodamine B dye) SWC Adsorbent Dye Adsorption Ref.

materials capacity
Langmuir paramters: (mg/g)
Q0, mg/g 18.52
b, I/mg 0.014 Coir pith carbon Rhodamine B 2.56 [2]
R2 0.9837 Coir pith carbon Acid violet 8.06 [2]
Sago waste Rhodamine B 16.12 [6]
Freundlich parameters: Waste coir pith Acid billiant 5.57 [7]
Kf, mg/g 3.28 blue
n 3.87 Waste coir pith Acid violet 7.34 [7]
R2 0.9578 Orange peel Rhodamine B 14.3 [26]
Orange peel Congo red 14.0 [26]
Orange peel Methyl violet 11.5 [26]
adsorption capacity and rate of adsorption, Orange peel Amido black 7.9 [26]
respectively. When Ce/qe was plotted against Ce, Banana peel Amido black 6.5 [26]
a straight line with slope 1/Q0 was obtained, Coir pith carbon Congo red 6.72 [28
indicating that the adsorption of RB on activated Parthenium Rhodamine B 18.52 This
carbon follows the Langmuir isotherm. The carbon study
Langmuir constants b and Q were calculated from
this isotherm and their values are given in
Table 2. rhodamine-B dye under conditions used in this
Confirmation of the experimental data with study. A list showing the adsorption capacity of
the Langmuir isotherm model indicates the homo- different adsorbents for the adsorption of differ-
geneous nature of SWC. The results also ent dye materials from their aqueous solution is
demonstrate the formation of monolayer coverage given in Table 3 where it is observed that the
of dye molecules at the outer surface of SWC. adsorption capacity of Parthenium carbon for dye
The essential characteristics of the Langmuir uptake is comparable with other low-cost
isotherm can be expressed in terms of a dimen- adsorbents.
sionless equilibrium parameter (RL) [23] which is
defined by: 3.5.2. Freundlich isotherm
The well-known logarithmic form of the
1 Freundlich model is given by the following
RL = (4) equation:
(1 + b ⋅ C0 )
log qe = log10 ( K f ) + (1/ n ) log 10 ( Ce ) (5)
where b is the Langmuir constant (1/mg) and C0
is the initial dye concentration (mg/L). The value where qe is the amount of dye adsorbed at equi-
of RL indicates the type of isotherm to be either librium (mg/g), Ce is the equilibrium concen-
unfavorable (RL >1), linear (RL = 1), favorable tration of adsorbate (RB) and Kf and n are the
(0< RL<1) or irreversible (RL = 0). The values of Freundlich constants. n gives an indication of
RL were in the range of 0 and 1, and confirmed how favorable the adsorption process and Kf is
that SWC is favorable for the adsorption of the adsorption capacity of adsorbent. Kf can be
258 H. Lata et al. / Desalination 219 (2008) 250–261

Fig. 6. Freundlich plot of log x/m vs. log Ce for

Rhodamine-B dye adsorption.

Fig. 7. Pseudo first-order kinetic plot for adsorption of

rhodamine-B dye on SWC.
defined as the adsorption or distribution coeffi-
cient and represents the quantity of dye adsorbed
t (min), respectively and k1 is the equilibrium rate
onto activated carbon adsorbent for a unit equi-
constant of pseudo-first-order sorption (1/min).
librium concentration. The slope 1/n ranging 0
The rate constant for the first-order equation was
and 1 is a measure of adsorption intensity or
determined from the slope of the plot log (qe!qt)
surface heterogeneity, becoming more hetero-
versus time. If first-order kinetics are applicable
geneous as its value gets closer to zero [24]. The
to the system under study, the plot of log (qe!qt)
plot of log qe versus log Ce gives a straight line
versus time of Eq. (6) should give a linear
with slope 1/n (Fig. 6), which shows that the
relationship. Further, the qe obtained from the plot
adsorption of rhodamine-B also follows the
should also be close to the qe obtained from the
Freundlich isotherm. Accordingly, the Freundlich
experimental at 150 mg/l dye concentration.
constants (Kf and n) were calculated and recorded
Fig. 7 shows that after a short period, the
in Table 2.
experimental data deviated considerably from
Table 2 shows the values of the parameter of
linearity. Even though the correlation coefficient
isotherms and the related correlation coefficients.
(R2) of the first-order equation is considerably
As seen from Table 2, the Langmuir model yields
high, the values of calculated qe from the first-
a somewhat better fit (R2 = 0.983) than the
order kinetic plot were far too small compared to
Freundlich model (R2 = 0.957).
the experimental values. The inapplicability of
the Lagergren equation to describe the kinetics of
3.6. Adsorption kinetic study rhodamine-B sorption was also observed by
Annadurai et al. for adsorption of dyes using
Kinetic adsorption data were treated with a
banana and orange peels [26]. The experimental
pseudo-first order kinetic model [25]:
data were also analyzed using the pseudo-second-
k1
log ( qe − qt ) = log qe −
order model [27]:
t (6)
2.303
t 1 1
where qe and qt refer to the amount of dye = 2
+ t (7)
adsorbed (mg g!1), at equilibrium and at any time, qt k2 qe qe
 H. Lata et al. / Desalination 219 (2008) 250–261 259

Table 4
Calculated and experimental qe values for different initial dye concentration

Initial qe, exp First-order kinetic model Second-order kinetic model SSE (%)
conc. (mg/l) (mg/g)

k1 qe, cal R2 SSE (%) k2 qe, cal R2

(1/min) (mg/g) (g/mg/min) (mg/g)

50 5.98 0.026 1.572 0.99 2.54 0.109 5.88 0.998 0.05

100 7.31 0.062 5.45 0.99 1.07 0.025 8.05 0.994 0.34
150 10.29 0.057 10.88 1 1.41 0.012 11.35 0.988 0.61
200 8.88 0.0267 1.442 0.71 4.48 0.033 9.65 0.993 0.38
250 10.80 0.0189 2.006 0.99 5.07 0.349 11.58 0.987 0.63

where k2 is the equilibrium rate constant of

pseudo-second-order adsorption (g mg!1min!1).
If pseudo-second-order kinetic is applicable to
the system under study, the plot of t/qt vs. time of
Eq. (7) should give a linear relationship. The
second-order sorption rate constant and qe were
determined from the slope and intercept of plot
t/qt vs. time for different initial dye concentra-
tions (Fig. 8). The correlation coefficients for the
linear plot are very high (>0.98) for almost all the
systems. The calculated qe values from the
pseudo-second-order model are in good agree-
ment with experimental qe values. This suggests Fig. 8. Pseudo-second-order kinetic plot for adsorption of
that the sorption system followed the pseudo- rhodamine-B by SWC.
second-order model. The values of kinetic con-
stants and qe values of rhodamine-B sorption onto
SWC are given in Table 4. the better the goodness of fit. The calculated
Beside the value of R2, the applicability of results are given in Table 4.
kinetic models are verified through the sum of
error squares (SSE, %). The adsorption kinetics
of RB on SWC was tested at different initial 4. Conclusion
concentrations. The validity of each model was Activated carbon prepared from parthenium
determined by sum of error squares (SSE, %) weed by chemical treatment, i.e., sulphuric acid
given by treated parthenium carbon (SWC) was used as an
adsorbent for the removal of rhodamine-B over a
∑ ( q , cal − q , exp )
2
SSE (%) = e e N (8) wide range of concentration. Dye removal from
aqueous solutions by SWC can be possible pro-
where N is the number of data points. The higher vided the initial dye concentration is low in the
the value of R2 and the lower the value of SSE, solution. Initial pH had no marked effect for
260 H. Lata et al. / Desalination 219 (2008) 250–261
rhodamine-B adsorption. The maximum removal
is practically achieved within 60 min. The equi-
librium data followed both the Langmuir and
Freundlich isotherm models. The kinetics of
rhodamine-B adsorption onto SWC followed the
pseudo-second-order model. These results indi-
cate that SWC could be used as a low-cost
material for dye removal from an aqueous
system.
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