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Removal of cadmium(II), lead(II),

and chromium(VI) ions from aqueous
solution using clay
a a
Tabrez A. Khan & Ved Vati Singh
a
Department of Chemistry , Jamia Millia Islamia , New Delhi 110
025, India
Published online: 19 Aug 2010.

To cite this article: Tabrez A. Khan & Ved Vati Singh (2010) Removal of cadmium(II), lead(II), and
chromium(VI) ions from aqueous solution using clay, Toxicological & Environmental Chemistry, 92:8,
1435-1446, DOI: 10.1080/02772241003592930

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 Toxicological & Environmental Chemistry
Vol. 92, No. 8, September 2010, 1435–1446

Removal of cadmium(II), lead(II), and chromium(VI) ions from

aqueous solution using clay
Tabrez A. Khan* and Ved Vati Singh

Department of Chemistry, Jamia Millia Islamia, New Delhi 110 025, India
(Received 19 July 2009; final version received 2 January 2010)
Downloaded by [Moskow State Univ Bibliote] at 02:00 14 November 2013

Removal of cadmium(II), lead(II), and chromium(VI) from aqueous

solution using clay, a naturally occurring low-cost adsorbent, under
various conditions, such as contact time, initial concentration, temperature,
and pH has been investigated. The sorption of these metals follows both
Langmuir and Freundlich adsorption isotherms. The magnitude of
Langmuir and Freundlich constants at 30 C for cadmium, lead, and
chromium indicate good adsorption capacity. The kinetic rate constants
(Kad) indicate that the adsorption follows first order. The thermodynamic
parameters: free energy change (DGo), enthalpy change (DHo), and entropy
change (DSo) show that adsorption is an endothermic process and that
adsorption is favored at high temperature. The results reveal that clay is a
good adsorbent for the removal of these metals from wastewater.
Keywords: adsorption; cadmium(II); lead(II); chromium(VI); clay;
Langmuir and Freundlich isotherms; thermodynamic parameters

Introduction
Pollution of water resources due to discharge of metal-laden aqueous effluents from
industrial units (Chuan et al. 2005; Tunali, Cabuk, and Akar 2006) is a serious
environmental concern. The health impact of metals such as cadmium (Cd), lead
(Pb), and chromium (Cr) when present beyond their permissible limits (3, 10, and
50 mg L1 for Cd, Pb, and Cr, respectively; WHO 2006) in drinking water is well
known. Cd is known to be carcinogenic to humans. Other adverse health effects
include lung insufficiency, bone lesions, cancer, and hypertension in humans.
Chronic Cd toxicity has also been the cause of the Japanese Itai-Itai disease.
High levels of Pb can cause severe dysfunction of the kidney, liver, central and
peripheral nervous system, anemia, and high blood pressure. The most severe neu-
rologic effect of Pb in adults is Pb encephalopathy, which is a general term to describe
various diseases that affect brain function. Lower IQ values and neuropsychologic
deficits among children are correlated to higher Pb levels (Marino et al. 1989). Cr(VI)
is highly toxic and is a source of various cancer diseases (Gil et al. 2006). It may cause
stomach irritation or ulceration, dermatitis, damage to nerve tissues, liver and kidney,

*Corresponding author. Email: takhan501@yahoo.com

ISSN 0277–2248 print/ISSN 1029–0486 online

ß 2010 Taylor & Francis
DOI: 10.1080/02772241003592930
http://www.informaworld.com
 1436 T.A. Khan and V.V. Singh

and even death at large doses (Kotas and Stasicka 2000). Therefore, the removal of
these toxic metals from industrial discharges is of utmost importance.
Various methods (Crini 2006) are available for removal of metal ions from
aqueous solution, including precipitation, membrane processes such as ultrafiltration
and reverse osmosis, ion exchange, and solvent extraction. Precipitation followed by
coagulation has limited applicability due to large volume of sludge being produced.
Membrane filtration is a proven way to remove metal ions but its high cost limits the
use in practice. Adsorption has been found to be a simple, efficient, and most
effective method for the removal of metal ions from wastewater. However, due to
high cost of conventional adsorbents such as activated charcoal, there is growing
interest in the use of low-cost, eco-friendly, and non-conventional adsorbents
(Ali and Gupta 2006). Many non-conventional adsorbents including industrial wastes
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(Gupta 1998; Gupta, Mohan, and Sharma 1998; Gupta et al. 1999; Gupta, Gupta,
and Sharma 2001; Gupta and Sharma 2002; Chakravarty et al. 2008; Khan, Singh and
Ali 2009), agricultural wastes and by-products (Gupta and Sharma 2003; Gupta and
Ali 2004; Tajar, Kaghazchi, and Soleimani 2009), and naturally occurring materials
(Gupta, Saini, and Jain 2005; Saltali, San, and Aydm 2007; San, Tuzen, and Soylak
2007; Eran 2008; Sen and Sarzali 2008; Sharma 2008; Kocaoba 2009; Shukla et al.
2009) have attracted the attention of several researchers. Recently, many
bio-adsorbents have been studied for the removal of Cd(II), Pb(II) and Cr(VI)
from aqueous solutions (Gupta, Srivastava, and Jain 2001; Gupta and
Bhattacharyya 2006a, 2006b; Gupta and Rastogi 2008a, 2008b, 2008c, 2008d, 2009).
Literature studies show that clay has remarkable capability for treatment of
contaminated wastewater (Ikhsan, Johnson, and Wells 1999; Coles and Yong 2002;
Sheta et al. 2003; Yavuz, Altunkaynak and Guzel 2003; Gupta and Bhattacharyya
2006a, 2006b). Clay is an important constituent of all soils. High specific surface
area, high porosity, chemical and mechanical stability, layered structure, and high
cation exchange capacity has made clay an excellent adsorbent with the capability to
adsorb positively charged species. Its sorption properties are a result of high surface
area and porosity (Alkan et al. 2004). The presence of both Bronsted and Lewis
acidity in clay boosts the adsorptive capacities.
In this article, we describe the results of our investigations on the use of clay as a
low-cost adsorbent for the removal of Cd, Pb, and Cr from aqueous solution.

Materials and methods

Cadmium nitrate, lead nitrate, potassium dichromate (Analytical Reagent grade,
Aldrich) were procured and used as such. Sulfuric acid and sodium hydroxide
(Analytical Reagent grade) were used as supplied. Absorbance studies were carried
out using a UV–visible spectrophotometer (Perkin Elmer Lambda EZ 201, MA,
USA). The pH measurements were done on a pH meter (Elico, LI 127, glass
electrode, Hyderabad, India). Stock solutions of Cd(II), Pb(II), and Cr(VI) were
prepared by dissolving cadmium nitrate, lead nitrate, and potassium dichromate,
respectively in double-distilled water. Standard solutions of Cd (2–12 mg L1),
Pb and Cr (5–30 mg L1) were prepared by diluting the stock solution. The pH of
the test solution was adjusted using dilute sulfuric acid and sodium hydroxide
(both 0.1 mol L1).
 Toxicological & Environmental Chemistry 1437

Adsorbent
Clay, a solid waste from Krishna–Pennar Link Canal Project, Karnataka
(SiO2, 44.21; Al2O3, 40.72; Fe2O3, 0.53; MgO, 0.12; Na2O, 0.014; K2O, 0.27; P2O5,
0.032 wt % and surface area, 12.7 m2 g1; porosity, 0.39; density, 2.57 g cm3) was
obtained from the Central Soil and Material Research Station, New Delhi, India.
The adsorbent was treated with hydrogen peroxide (100 volumes) at 60 C until
bubbling stopped within 24 h, indicating the complete oxidation of adhering organic
impurities. The resulting product was washed with distilled water, dried in an oven at
110 C for 24 h, finely crushed and sieved through 75, 150, 300, and 425 mm sieves,
and kept in separate plastic bags in a vacuum desiccator until required for adsorption
studies. For the adsorption experiments, the fraction with a particle size of 75 mm was
selected because of its high adsorption capacity.
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Adsorption studies
Batch adsorption studies were carried out using Cd(II), Pb(II), and Cr(VI) solutions
of desired concentrations in glass bottles (50 mL) containing accurately weighed
amounts (1 g) of adsorbent. The bottles were shaken at 20, 30, and 40 C using
constant temperature water bath shaker for a predetermined span of time to attain
equilibrium. The adsorbent was then removed by centrifugation at 3500 rpm.
The supernatant solution was analyzed for its residual metal content spectro-
photometrically (APHA 1985). The kinetics of the adsorption of metal ions on clay
was evaluated using a procedure similar to that used in the adsorption experiments.
The batch experiment was repeated at different time intervals using 1 g adsorbents
and 50 mL solution at pH 5.5 for Cd and Pb, and at pH 2.5 for Cr at 20, 30, and
40 C. For equilibrium studies, adsorption studies were conducted at the following
metal ion concentrations (2–12 mg L1, pH 5.5 for Cd; 5–30 mg L1, pH 5.5 for Pb;
5–30 mg L1, pH 2.5 for Cr) at 20, 30, and 40 C.
All experiments were carried out in triplicate to test reproducibility, achieving a
relative deviation in the order of 0.5–2.5%. Blanks were run without adsorbents
under similar conditions of concentration, pH, and temperature, to correct for any
adsorption onto the internal surface of the glass bottles.

Results and discussion

The effect of contact time on the uptake of the studied metal ions (10 mg L1, 30 C)
onto clay was studied by varying the contact time from 20 to 180 min. The amount of
metal ions removed by clay as a function of time is presented in Figure 1. Adsorption
of metal ions increases rapidly between 20 and 60 min becoming slower when
approaching saturation. Equilibrium was attained within 110 min for Cd(II), Pb(II),
and Cr(VI). The same equilibration time indicates a similar affinity of clay for the
tested metals. At equilibrium, the removal percentage varied in the order Cd
(97%)4Pb (88%)4Cr (87%).
The kinetic rate constant (Kad) for adsorption was determined using Lagergren’s
first-order rate expression (Ho 2004; Sharma 2008). The Kad values (min1) at 30 C
for Cd (4.60  102), Pb (3.46  102), and Cr (3.63  102) were calculated from the
slopes of the linear plots of log(qe  qt) versus time (t) (Figure 2). The high
correlation coefficients (R2 ¼ 0.98–0.94) indicate that adsorption follows first-order
rate kinetics.
 1438 T.A. Khan and V.V. Singh

0.60
Cadmium 2 mg L–1
4 mg L–1

Amount adsorbed (mg g–1)

6 mg L–1
8 mg L–1
0.40 10 mg L–1
12 mg L–1

0.20

0.00
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0 50 100 150 200

Time (min)

1.60
Lead 5 mg L–1
1.40
Amount adsorbed (mg g–1)

10 mg L–1
15 mg L–1
1.20 20 mg L–1
1.00 25 mg L–1
30 mg L–1
0.80
0.60
0.40
0.20
0.00
0 50 100 150 200
Time (min)

1.60
Chromium 5 mg L–1
1.40 10 mg L–1
Amount adsorbed (mg g–1)

15 mg L–1
1.20 20 mg L–1
25 mg L–1
1.00 30 mg L–1

0.80

0.60

0.40

0.20

0.00
0 50 100 150 200
Time (min)

Figure 1. Effect of concentration on the adsorption of metal ions.

The pH of the solution is one of the most important parameters affecting the
adsorption process since it governs the surface charge of the adsorbent and the
chemistry of the metal ions. The effect of pH on the removal of metal ions
(10 mg L1) by the clay (1 g) is shown in Figure 3. As the pH of the solution increases
 Toxicological & Environmental Chemistry 1439

–0.60
Cadmium

–1.60

log (qe–q)
–2.60

–3.60
20° C
30° C
–4.60
40° C

–5.60
0 20 40 60 80 100 120
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Time (min)

–0.60
Lead

–1.60
log (qe–q)

–2.60

–3.60

–4.60

–5.60
0 20 40 60 80 100 120
Time (min)

–0.60
Chromium

–1.60
log (qe–q)

–2.60

–3.60

–4.60

–5.60
0 20 40 60 80 100 120
Time (min)

Figure 2. Adsorption kinetic plots for metal ions removal at different temperatures.

from 1 to 6, the percent adsorption of Cd and Pb increases from 47 to 88, and from
58 to 93, respectively, indicating optimum adsorption at pH 5.5. However, in the case
of Cr, the percent adsorption increases from 85 to 94 when the pH is increased from
1 to 3, with optimum adsorption occurring at pH 2.5. The results indicate that
adsorption process may favorably be used for the removal of Cr from acidic effluents
(like electroplating wastes), while prior pH adjustment is necessary for neutral or
alkaline effluents.
 1440 T.A. Khan and V.V. Singh

0.50

Amount adsorbed (mg g–1)

0.40

0.30

Cadmium
0.20
Lead

Chromium
0.10
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0 2 4 6 8 10 12
pH

Figure 3. Effect of pH on the adsorption of metal ions.

Based on these results, the increased binding of Cd and Pb to clay with increasing
pH may be explained on the basis of the type and ionic state of the functional groups
present on the clay surface, which due to their ability to interact with metal ions is
likely to be the active site for metal adsorption. At lower pH (53), these sites are
occupied by hydronium ions (H3Oþ) resulting in restricted access of metal ions
because of repulsive forces. As the pH increases, H3Oþ ions are released and the
number of active sites available for interaction with metal ions increases. In this pH
range, it is believed that ion exchange and complex formation are the major
mechanisms for removal of metal ions from solution (Jain and Ram 1997; Coles and
Yong 2002).
The variation in adsorption of Cr with increasing pH suggests improved binding
to the adsorbent with an optimum at pH 2.5. This may be ascribed to the availability
of positively charged active sites on the adsorbent surface at low pH (53) for
2
interaction with predominant negatively charged species of Cr (HCrO 4 , Cr2 O7 ,
2 2
Cr3 O10 , and Cr4 O13 ). The Cr–clay binding, thus, appears to be ion exchange
involving electrostatic attraction. Above pH 3, the rate of Cr removal is considerably
lower (Figure 3). It seems that in this pH range, the clay surface carries a net negative
charge that tends to repel the anions. Hence, it appears that above pH 3,
the mechanism of adsorption of Cr onto the adsorbent is largely physical (Rao, Mise,
and Manjunatha 1992; Jain and Ram 1997; Selvi, Pattabhi and Kadirvelu 2001;
Dakiky et al. 2002; Leyva-Romos, Bernal-Jacome, and Acosta-Rodriguez 2005).
Experiments on the effect of different initial metal concentrations were carried out
with Cd, 2–12 mg L1, Pb, and Cr, both 5–30 mg L1, at 30 C. It was found that with
increased initial metal ion concentrations, adsorption per unit weight of adsorbent
increases (Figure 1), while the percentage removal decreases from 91 to 87% for
Cd(II), from 94% to 92% for Pb(II), and from 95% to 93% for Cr(VI). The decrease
in percentage of metal uptake may be explained by the fact that all adsorbents have
limited numbers of active sites that become saturated above a certain metal
concentration (Ulmanu et al. 2003; Zheng et al. 2008).
The adsorption capacities were evaluated by Langmuir and Freundlich isotherm
models (Gupta and Rastogi 2008). A linear plot of Ce/qe versus Ce (Figure 4)
indicates that Langmuir equation is obeyed. The Langmuir constant, Qo, which
 Toxicological & Environmental Chemistry 1441

6 Cadmium

Ce/qe
3

2 20° C
30° C
1 40° C

0
0 1 2 3
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Ce
5
Lead

3
Ce/qe

0
0 1 2 3 4 5
Ce
5
Chromium
4

3
Ce/qe

0
0 1 2 3 4 5
Ce

Figure 4. Langmuir plots for the adsorption of metal ions at different temperatures.

denotes the quantity of adsorbate forming a monolayer coverage on the unit mass of
adsorbent (mg g1), and b, which denotes adsorption energy, are calculated from the
slope and intercept of Langmuir plots, respectively (Table 1). Both these parameters
increase with increased temperature indicating an endothermic nature of the adsorp-
tion process. High correlation coefficients (R2) show good correlation (0.95–0.99).
 1442 T.A. Khan and V.V. Singh

Table 1. Constant values of Langmuir and Freundlich isotherms for adsorption of metal ions
onto clay at different temperatures.

Langmuir constants Freundlich constants

Adsorbate Temperature
(Metal ions) ( C) Qo (mg g1) b (L mg1) KF (mg g1) 1/n

Cd(II) 20 1.45 0.199 0.234 0.831

30 1.48 0.345 0.373 0.821
40 1.50 0.817 0.752 0.809
Pb(II) 20 3.20 0.131 0.368 0.794
30 3.44 0.249 0.658 0.795
40 3.53 0.413 1.010 0.804
Cr(VI) 20 3.31 0.196 0.521 0.799
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30 3.47 0.290 0.747 0.794

40 3.56 0.621 1.417 0.807

The dimensionless separation factors, RL, known as reliable indicators of adsorption

(Dogan and Alkan 2003), at different temperatures are in the range from 0.026 to
0.025 for Cd(II), from 0.043 to 0.012 for Pb(II), and from 0.004 to 0.018 for Cr(VI).
RL values between 0 and 1 indicate favorable adsorption.
The results obtained with the Freundlich model using a linear plot of log qe versus
log Ce (Figure 5) indicate its applicability (Gupta and Bhattacharyya 2006a, 2006b).
Freundlich constants, KF (indicating adsorption capacity), and 1/n (adsorption
intensity) calculated from the slopes and intercepts of the Freundlich plots are
tabulated in Table 1. The high correlation coefficients (R2) of 0.99–0.98 indicate that
the data fit reasonably well to the Freundlich isotherm.
The studies of the effect of temperature on adsorption are important because it
affects the rate and extent of adsorption and provides information about adsorbate–
adsorbent interaction. Experiments were performed at 20, 30, and 40 C at a concen-
tration of 10 mg L1. The extent of adsorption increased from 82 to 96% for Cd(II),
from 88% to 97% for Pb(II), and from 89% to 98% for Cr(VI) with rise in
temperature from 20 C to 40 C. The results indicate that the adsorption process is
endothermic which is consistent with diffusion-controlled adsorption. At higher
temperature, the adsorbate transport is facilitated, apart from an increase in the
number of adsorption sites generated due to breaking of some internal bonds near
the edge of active surface.
The standard free energy change (DGo), enthalpy change (DHo), and entropy
change (DSo) are calculated (Sharma 2008). The DGo values are in the range from
24.4 to 29.8 for Cd(II), from 23.4 to 27.8 for Pb(II), and from 22.5 to 27.0 kJ mol1
for Cr(VI). The values of DGo being more negative with increase in temperature
show that the removal process is favored at high temperature (Khan, Rehman, and
Khan 1995). Positive values of DHo [40.5–68.2 for Cd(II), 47.7–39.9 for Pb(II), and
28.7–60.2 kJ mol1 for Cr(VI)] between 20 C and 40 C show that the adsorption
process is endothermic in nature (Ho and McKay 1999). The increase in DSo values
with increasing temperature [from 221 to 313 for Cd(II), from 242 to 216 for Pb(II),
and from 175 to 278 J K1 mol1 for Cr(VI)] shows an increase in randomness at the
solid–liquid interface during the adsorption process.
 Toxicological & Environmental Chemistry 1443

1.00
Cadmium
0.00

log qe
–1.00

20° C
–2.00 30° C
40° C
–3.00
–3.00 –2.00 –1.00 0.00 1.00 2.00
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log Ce
1.00
Lead

0.00
log qe

–1.00

–2.00

–3.00
–3.00 –2.00 –1.00 0.00 1.00 2.00
log Ce
1.00
Chromium

0.00
log qe

–1.00

–2.00

–3.00
–3.00 –2.00 –1.00 0.00 1.00 2.00
log Ce

Figure 5. Feundlich plots for the adsorption of metal ions at different temperatures.

Conclusions
The results indicate that clay, a naturally occurring low-cost adsorbent, can
effectively be used for removal of Cd(II), Pb(II), and Cr(VI) from aqueous
solution. The equilibrium data fitted well both to Langmuir and Freundlich
isotherms. The adsorption process followed the Lagergren first-order rate equation.
The thermodynamic parameters (DGo, DHo) showed that the adsorption of metal
 1444 T.A. Khan and V.V. Singh

ions onto clay is favorable, spontaneous, and endothermic in nature. Positive values
of DSo suggest an increase in randomness.

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