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Journal of Colloid and Interface Science 396 (2013) 264269

Contents lists available at SciVerse ScienceDirect

Journal of Colloid and Interface Science

www.elsevier.com/locate/jcis

Adsorption of lead ions from aqueous solution using porous carbon derived
from rubber tires: Experimental and computational study
Tawk A. Saleh a, Vinod K. Gupta a,b,, Abdulaziz A. Al-Saadi a
a
b

Department of Chemistry, King Fahd University of Petroleum & Minerals, Dhahran, Saudi Arabia
Chemistry Department, Indian Institute of Technology Roorkee, Roorkee 247 667, India

a r t i c l e

i n f o

Article history:
Received 5 December 2012
Accepted 17 January 2013
Available online 31 January 2013
Keywords:
Porous carbon
Lead ion removal
FT calculations

a b s t r a c t
Effective activated porous carbon (AC) was prepared by thermal treatment of waste rubber tires and was
further activated using oxidizing agents like nitric acid and hydrogen peroxide. The tire-derived porous
carbon was characterized by means of FTIR and X-ray diffraction. Careful analysis of the IR spectra of the
synthesized AC reveals a number of bands centered at about 3400, 2350, 1710, 1650, and 1300
1000 cm1, proving the existence of hydroxyl and carboxylic groups on the surface of AC in addition to
C@C double bonds. The developed AC was tested and evaluated as a potential adsorbent for the removal
of lead (II) ions. Experimental parameters, such as contact time, initial concentration, adsorbent dosage,
and pH were optimized. AC was effective in a pH range between 4 and 7 with a highest uptake of lead
ions at pH 5 and 6. For further understanding of the chemistry behind the process, density functional theory (DFT) calculations were performed at the B3LYP/6-31G(d) level adopting a functionalized pyrene
molecule as a model. The binding energy of Pb(II) ion toward carboxylic acid, carbonyl, and hydroxyl
groups was calculated. A binding energy in the range of 310340 kcal/mol, which is considered to be high
and to be indicative of a chemisorptions process, was predicted. The adsorption of the lead ion toward the
C@O groups in relatively all cases shows more stable binding compared to the sorption toward the alcohol groups.
2013 Elsevier Inc. All rights reserved.

1. Introduction
Contamination of the environment from different activities has
become an increasingly serious problem in recent years. Heavy
metals are one class of toxic pollutants released into the surface
and ground water as a result of various activities such as industries, mining, and agriculture [1]. The rapid development of industry has led to severe problems of water pollution. Industries and
municipal authorities have been forced to treat wastewater before
discharging. Various methods are available for water treatment.
However, adsorption technology is considered as an efcient and
universal method of water treatment as per the guidelines of
WHO and EPA. This is because of its cost effectiveness and environmental friendliness. The cost effectiveness of this technology is due
to the use of effective adsorbents by converting solid waste to value-added products.
Tire rubber is a mixture of different elastomers such as natural
rubber, butadiene rubber, and styrene butadiene rubber plus other
additives like carbon black, sulfur, and zinc oxide. Approximately

Corresponding author at: Chemistry Department, Indian Institute of Technology

Roorkee, Roorkee 247 667, India. Fax: +91 1332286202.
E-mail address: vinodfcy@gmail.com (V.K. Gupta).
0021-9797/$ - see front matter 2013 Elsevier Inc. All rights reserved.
http://dx.doi.org/10.1016/j.jcis.2013.01.037

32% by weight of the waste tire is mainly constituted of carbon

black in which the carbon content is as high as 7075 wt.% [24].
The increase in waste rubber tires and other rubber materials
imposes serious threats on the public health and safety as well
as environment. Different methods are used for rubber disposal
including grinding which converts it into granulates used as ller
for thermoplastics [57]. One potential application for the waste
rubber tire char is to produce activated carbon (AC) which is used
as adsorbent. AC is of high porosity and high surface area material
manufactured by carbonization and activation of carbonaceous
materials by either physical or chemical activation methods [8,9].
Water pollution by heavy metals is considered a serious menace
to the environment and especially to human health [10]. According
to the World Health Organization, the most common toxic metals
found in wastewater are lead, copper, cadmium, chromium, zinc,
and nickel. Lead is widely used in processing industries such as
electroplating, paint and dyes, explosive manufacturing, and lead
batteries [11]. The presence of lead ion in water even at a very
low level, 5 ng mL1, would be harmful to aquatic life and endanger human health because of its toxicological, potential carcinogenic, and neurological effects [12].
The maximum permissible limit (MPL) of lead in drinking water
is 0.1 mg/L according to the World Health Organization since lead
is cumulative poison [13]. Hence, the appropriate treatment of

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T.A. Saleh et al. / Journal of Colloid and Interface Science 396 (2013) 264269

industrial wastewater which releases lead into the aquatic and terrestrial systems is very important. Various adsorbents have been
reported for the removal of metal ions and organic compounds
from waters [1444]. Most of these adsorbents might not be efcient in removing heavy metal at very low concentrations and
could be relatively expensive. Therefore, it is essential to further
activate the adsorbent surface to enhance adsorption capacity.
The objective of the present study was to prepare activate porous carbon from waste rubber tire with a combination of physical
and chemical treatment in an attempt to develop surface porosity
as well as to incorporate desired functional groups on the surface
of the resultant activated carbon. The adsorption capacity of the
developed carbon was further evaluated for lead ions removal from
waste water. Factors that are likely to affect the adsorption capacity of the developed carbon were studied. In addition, a computational study was conducted.
2. Experimental section

265

FTIR 180 spectrophotometer using KBr pellets over the range

4000400 cm1. For the FTIR study, 10 mg of nely sized particle
of the adsorbent was encapsulated in 300 mg of KBr keeping the
ratio 1:30, in order to prepare the translucent sample disks.
2.4. Adsorption and kinetic studies
The kinetic and isothermal studies were performed using a series of 250-mL Erlenmeyer asks which were lled with 100 mL
lead solution of varying concentrations (120 ppm), maintained
at desired temperature and pH. The pH of the solution was kept
constant by adding 0.2 M NaOH or 0.2 M HNO3. An equal amount
of adsorbent was added separately into each individual ask. The
asks were agitated in a thermostatted shaker at a speed of
150 rpm. Liquid samples were taken out at a given time interval
and centrifuged at 1500 rpm for 3 min. The concentration of
remaining lead ions in the adsorption medium was determined
by the ICP-MS. The adsorption capacity for lead ions uptake, qe
(mg/g), was determined using the following equation:

2.1. Reagents

qe C 0  CV=W

Nitric acid and lead nitrate were obtained from SigmaAldrich.

Stock solutions of the lead ions were prepared in deionized water
(the resistance of the deionized water is 0.5 lS). Lead solutions of
different initial concentrations were prepared by diluting the stock
solution in appropriate proportions. In order to prevent metal contamination from laboratory glassware, glassware was kept overnight in a 10% (v/v) HNO3 solution. Safety precaution was
considered in handling all chemicals and conducting the experimental work [45,46]. All reagents used in the study were of analytical grade.

and the percentage of removal was calculated using the following

equation:

%removal C 0  C=C  100

where C0 and C are the initial and nal lead concentrations (ppm),
respectively, V is the volume of solution (L) and W is the weight
of adsorbent (g). All the experiments were repeated three times,
and average values were reported. The standard deviation was
found to be 0.2%; values of the correlation coefcient averaged 0.99.
The parameters considered for study were initial concentration
of adsorbate, contact time, adsorbent dose, pH, and temperature.

2.2. Development of the adsorbent

2.5. Computational part
Waste rubber tire is cleaned and ground. The tire granules were
heated up to 300 C to separate the produced oil; black tire crude
oil and yellow distilled diesel oil. Then, thermal pyrolysis was performed at a temperature of around 500 C for 3 h in the presence of
helium to break down the cross-linkage between carbon atoms.
The activation process was performed using steam as activating
gas at 900 C for 2 h, for further development of the porosity of tire
carbon [47].
Further modication was accomplished via HNO3 and H2O2
treatment in order to develop oxygen surface groups on the rubber
tire carbon. For this purpose, the product was treated with HNO3
(4 M concentration) with a ratio of 1 g of carbon to 20 mL of
HNO3 [48]. The mixture (carbon and acid solution) was stirred
and heated at 60 C for 24 h. Then, it was washed thoroughly and
dried at 100 C. After that, the product was treated with H2O2
(6% concentration) with a ratio of 1 g/20 mL carbon/H2O2. The mixture (carbon and acid solution) was stirred and heated at 60 C for
24 h. Then, it was washed thoroughly and dried at 100 C which
was then be characterized. This is referred to as RAC throughout
the study.
2.3. Characterization of activated carbon
The activated carbon produced from waste rubber tires (RAC)
was characterized by means of scanning electron microscope (FESEM, FEI Nova-Nano SEM-600, Netherlands) for scanning the adsorbent surface and energy-dispersive X-ray spectroscopy (EDX) for
the quantitative analysis of the components of RAC. Fourier transform infrared spectroscopy (FT-IR) was used for identifying types
of chemical bonds and functional groups and oxygen containing
groups. The IR spectra of the RAC were recorded on a PerkinElmer

The representative calculations for Pb(II) ion adsorption on several functionalized pyrene systems have been carried out with the
G09 program package14 utilizing the DFT-B3LYP method with the
6-31+G basis set for H, C and O atoms and the SDD pseudo-potential for Pb(II) ion. Full geometry optimizations were performed on
the models shown in Fig. 8 without any constraint. The stationary
points have been conrmed by frequency calculation, and the initial binding energy was predicted from the following equation:

BEPbPyr EPyr EPbII  EPbPyr

3. Results and discussion

3.1. Characterization of RAC
The morphology of the activated carbon produced from waste
rubber tires was characterized by SEM, Fig. 1. The SEM image
shows the porous structure of the activated carbon. The image
exhibits two distinct morphologies. One of the morphological regions is granular in nature (the granules are 0.5 lm in diameter),
and a large number of the granules can be observed in the image.
High resolution of the image of the developed activated carbon
indicates that there are different pore structures in the adsorbent.
The basic parameters for an effective adsorbent are high surface
area and pore structure. When the porosity increases, the surface
area also increases [4951].
EDX measurements were conducted for the compositional analysis of the RAC. The spectrum in Fig. 2 conrms the presence of carbon and oxygen in the tire-derived carbon. Table 1 presented the
EDX quantitative microanalysis of the tire-derived carbon.

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Fig. 4. Effect of lead initial concentrations on the adsorption on the tire-derived

activated carbon. (Conditions: initial lead concentration = variable; dosage of
adsorbent = 0.5 mg; pH 5; agitation speed = 150 rpm; contact time = 80 min.)

Fig. 1. SEM image of the surface structure of the tire-derived activated carbon.

The IR spectra of the tire-derived activated carbon were measured by recorded on a PerkinElmer FTIR 180 spectrophotometer
using KBr pellets over the range 4000400 cm1. The spectrum,
not shown, displays a number of bands. The assignment of the carbonyl band to an ester is conrmed by observation of a strong band
in the CAO stretching region at about 1180 cm1 (broad band
11001300 cm1) [52]. The band at 1580 cm1 is attributed to
C@C double bonds [53]. The carboxylic acid group is usually presumed to take part in the adsorption of metal ions from aqueous
solution [54]. The bands at 1710 and 1650 cm1 are ascribable in
turn to stretching (m) (C@O) vibrations of carboxyl and carbonyl
in acidic oxygen surface groups. The band at 3400 cm1 is attributed to stretching (OAH) vibration in hydroxyl groups. The band
at 2350 cm1 is attributed to CC stretching vibration of the alkyne group [55].

Fig. 2. EDX spectrum of activated carbon derived from the tire.

3.2. Experimental parameters

Table 1
Energy dispersive X-ray analysis (EDX) quantitative microanalysis
of the tire-derived activated carbon.
N#

Element

Weight%

Atomic%

1
2

CK
OK
Total

93.95
6.05
100.00

95.39
4.61

3.2.1. Effect of contact time

In order to establish the rate of metal removal and the equilibrium time for maximum uptake and to know the kinetics of the
sorption process, the adsorption of lead ions by developed activated carbon was carried out under contact times from 0 to
140 min, Fig. 3. The adsorption efciency of lead ions increases
gradually with increasing contact times and reaches equilibrium
at around 80 min at which point the majority of Pb(II) is removed.
At this point, the amount of lead being adsorbed onto the RAC was
in a state of dynamic equilibrium with the amount of lead desorbed from the adsorbent. According to the results, the equilibrium
time is xed at this time for the rest of the batch experiments to
make sure that equilibrium is reached.
3.2.2. Effect of lead initial concentrations
The effect of the initial concentration of lead ions on the adsorption process was also investigated. The removal extent of lead is
dependent on the initial concentration. This is reasonable since
the more the lead ions available in the solution, the faster the
adsorption due to the enhancement in the dynamic contact between the adsorbent and the adsorbate. As depicted in Fig. 4, the
uptake slightly increases by decreasing the initial lead concentration which indicates perhaps that at higher concentration rates,
equilibrium is not attained in 80 min.

Fig. 3. The effect of contact time on the amount of lead ions adsorbed on the tirederived activated carbon. (Conditions: initial lead concentration 20 ppm; dosage of
adsorbent = 0.5 mg; pH 5; agitation speed = 150 rpm; contact time = variable.)

3.2.3. Effect of agitation speed

The agitation speed is considered an important parameter in the
adsorption process. The agitation speed was varied between 0 and

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150 rpm keeping all other experimental variables (initial lead concentration 20 ppm; dosage of adsorbent = 0.5 mg; pH 5; contact
time = 80 min) constant. It was observed that the percentages of
lead adsorbed increased as the agitation speed was increased,
Fig. 5. The removal ratio of lead increased from about 25% to
around 85% by increasing the speed between 20 and 150 rpm.
The adsorption capacity was greatest when agitation speed of
120 and 150 rpm was used. Fig. 5 shows that the extent of adsorption is not independent of agitation rate until the latter exceeds
120 rpm. Thus, at slower agitation rates, equilibrium is not attained in 80 min.

3.2.4. Effect of adsorbent dosage

The dose of adsorbent (m) was varied from 0.0 to 1.0 g/L, keeping all other experimental variables constant. As depicted in Fig. 6,
the percentage of lead removal increases up to adsorbent dose of
1 g/L. This may be attributed to an increased sorbent surface area
and availability of more adsorption sites resulting from the increased dose of the adsorbent. The percentage of removal of Pb(II)
increases from 15% to 85% with an increase in the amount of adsorbent from 0.1 to 0.5 g, respectively.

3.2.5. Effect of the pH

The effect of the pH value of the solution is an important controlling parameter in the adsorption process. It inuences both

the adsorbent surface metal binding sites and the metal chemistry
in water [56].
As a function of solution pH, Pb2+ is the dominant species below
pH value of about 6. Between pH 6 and 8, Pb undergoes hydrolysis to
Pb(OH)+. Above pH 9, solid lead hydroxide Pb(OH)2 is thermodynamically the most stable phase, while PbOH
3 is predominant at
pH above 11 [57,58]. In order to nd the optimal pH value for the
sorption process, the pH of feed solution was examined using solutions of different pH levels, covering a range of 2.09.0. At
pH > 7.0, the Pb(II) gets precipitated due to hydroxide anions
forming a lead hydroxide precipitate. As shown in Fig. 7, the range
between 2 and 7 was chosen to avoid metal solid hydroxide precipitation. The results indicate that the removal of lead ions onto the
activated carbon is pH dependent. At low pH range between 2.0
and 3.0, hydrogen ions compete with lead ions for the surface of
the adsorbent which would hinder Pb(II) ions from reaching the
binding sites of the sorbent caused by the repulsive forces. The
increase in metal removal as pH increases to 4 can be explained on
the basis of a decrease in competition between protons (H+) and
positively charged metal ions at the surface sites. The maximum
uptake of lead ions is obtained at pH 5 and 6 with highest efciency
of 85%. This can be explained by the point of zero charge of the
developed activated carbon which was measured and found to be
at 4.5 (pHpzc = 4.5). According to the Pb(II) speciation diagram and
in this range of pH, the dominant species of sorption are Pb2+ [59].
At pH of 5 or 6, the adsorbent surface is negative and the lead presents as Pb2+ which reect the electrostatic adsorbate/adsorbent
interactions.
3.3. Computational study
For further understanding of the chemistry behind the process,
density functional theory (DFT) calculations were performed at the

Fig. 5. The effect of agitation speed on the amount of lead adsorbed on the tirederived activated carbon. (Conditions: initial lead concentration 20 ppm; dosage of
adsorbent = 0.5 mg; pH 5; agitation speed = variable; contact time = 80 min.)

Fig. 7. The effect of pH on the amount of lead adsorbed on the tire-derived

activated carbon. (Conditions: initial lead concentration 20 ppm; contact time =
80 min; dosage of adsorbent = 0.5 mg; pH = variable; agitation speed = 150 rpm.)

Table 2
Binding energies (kcal/mol) and bond distances (angstroms) of the adsorption of
mono-binding lead ion on functionalized pyrenes as calculated at the B3LYP/6-31+G
level of theory.
Site type

Fig. 6. The effect of dosage on the amount of lead ions adsorbed on the tire-derived
activated carbon. (Conditions: initial lead concentration 20 ppm; dosage of adsorbent = variable; contact time = 80 min; pH 5; agitation speed = 150 rpm.)

Pyr-COOH
Pyr-C@O
Pyr-OH
Pyr-COOH

BE (kcal/mol)

Bond distance ()

Ecorrected

337
333
330
319

337
334
329
319

2.446
2.185
2.498
2.519

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Fig. 8. Optimized models of mono-binding of Pb(II) ion with (a) carbonyl oxygen of the carboxylic acid, (b) carbonyl oxygen, (c) alcoholic oxygen, and (d) alcoholic oxygen of
the carboxylic acid.

B3LYP/6-31+G level. The initial binding energy of Pb(II) ion toward

carboxylic acid (two possible positions), carbonyl, and hydroxyl
groups was calculated Fig. 8, and results are listed in Table 2. A
binding energy in the range of 310340 kcal/mol was predicted.
It is considered to be relatively high and indicative of a possible
chemisorption process. The adsorption of the lead ion toward the
C@O groups in relatively all cases shows more stable binding compared to the sorption toward the alcohol groups. In the case of a
purely carbonyl group, the lead ion tends to approach much closer
and more conveniently toward the carbonyl oxygen atom compared to the other cases. The initial binding energy, yet, seems to
be in this case more sensitive toward the nature of the functional
group rather than the proximity of the lead ion to the binding site.
4. Conclusion
Waste rubber tires were converted into a carbonaceous adsorbent and used for the removal of aqueous lead from wastewater.
The activation process facilitated in the incorporation of carbonyl
and hydroxyl functional groups onto the adsorbent surface; these
ultimately helped in the adsorption process. Further, this has been
supported by the density functional theory (DFT) calculations,
which indicate the high binding energy (310340 kcal/mol) of
Pb(II) ion toward carboxylic acid, carbonyl, and hydroxyl groups,
respectively.
On the basis of the results obtained, it can be safely concluded
that the AC developed from waste rubber tires act as potential
adsorbents for the removal of lead ions from aqueous media.
Waste rubber tires are a cheap and easily available material that
thus can act as a better replacement source for commercial AC.
Being a waste product, the use of waste rubber tires as adsorbent
would also solve their disposal problem.
Acknowledgments
The authors would like to acknowledge the support provided by
King Abdulaziz City for Science and Technology (KACST) through

the Science & Technology Unit at King Fahd University of Petroleum & Minerals (KFUPM) for funding this work through Project
No. 10-WAT1400-04 as part of the National Science, Technology
and Innovation Plan.

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