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Chromium removal by combining the magnetic properties of

iron oxide with adsorption properties of carbon nanotubes

V.K. Gupta a,b,*, Shilpi Agarwal b, Tawfik A. Saleh a

a
Chemistry Department, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia
b
Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India

article info abstract

Article history: The adsorption features of multiwall carbon nanotubes (MWCNTs) with the magnetic
Received 1 July 2010 properties of iron oxides have been combined in a composite to produce a magnetic
Received in revised form adsorbent. Composites of MWCNT/nano-iron oxide were prepared, and were characterized
12 January 2011 by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and
Accepted 15 January 2011 Fourier transform infrared spectroscopy (FTIR). XRD suggests that the magnetic phase
Available online 22 January 2011 formed is maghemite and/or magnetite. FESEM image shows nano-iron oxides attached to
a network of MWCNTs. The adsorption capability of the composites was tested in batch
Keywords: and fixed bed modes. The composites have demonstrated a superior adsorption capability
Multi-wall carbon nanotube/nano- to that of activated carbon. The results also show that the adsorptions of Cr(III) on the
iron oxide composite composites is strongly dependent on contact time, agitation speed and pH, in the batch
Chromium mode; and on flow rate and the bed thickness in the fixed bed mode. Along with the high
Fixed bed surface area of the MWCNTs, the advantage of the magnetic composite is that it can be
Batch mode used as adsorbent for contaminants in water and can be subsequently controlled and
XRD removed from the medium by a simple magnetic process.
SEM ª 2011 Elsevier Ltd. All rights reserved.
FTIR

1. Introduction (Rana et al., 2004; Rutland, 1991). According to EPA drinking

Heavy metals like Cr, Pb, Hg and Cd are common pollutants in
environment. Chromium, one of these metals exists in two
stable oxidation states, Cr (III) and Cr (VI). Chromium remains
the sole leather-tanning chemical since its first successful
trial by an American dye chemist, Augustus Schultz, in his
two-bath method (Stellmach, 1990). Tanneries use basic
chromium sulfate (CrOHSO4), which contains chrome in the
trivalent oxidation state. Other main sources of chromium
pollution are mining; cement ceramics and glass industries,
uses in dyes, electroplating, and production of steel and other
metal alloys, photographic material and corrosive paints
water standards, the maximum limit of chromium in drinking
water is 0.1 mg/L which is based on total chromium (US EPA,
2011). The presence of strong oxidants can change Cr (III) to
Cr (VI) (Tadesse et al., 2006).
Various naturally available adsorbents like wool, olive cake,
sawdust, pine needles, almond shells, cactus leaves, charcoal
used tyres, soot, hazelnut shell, coconut shell charcoal, banana
peel, seaweed, dead fungal biomass, cyanobacterium, and
green alga were used for the removal of chromium (Gupta et al.,
1999, 2001; Gupta and Ali, 2004; Ali and Gupta 2007; Gupta and
Rastogi, 2008, 2009; Gupta et al., 2009; Singh et al., 2007).
However, many of these naturally available adsorbents have

* Corresponding author. Chemistry Department, Indian Institute of Technology Roorkee, Roorkee 247667, India.
Tel.: þ91 1332 285801; fax: þ91 1332 273560.
E-mail address: vinodfcy@gmail.com (V.K. Gupta).
0043-1354/$ e see front matter ª 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.watres.2011.01.012
2208 w a t e r r e s e a r c h 4 5 ( 2 0 1 1 ) 2 2 0 7 e2 2 1 2
low chromium adsorption capacity and slow process kinetics.
Thus, there is a need to develop innovative adsorbents useful
both for industry and for the environment.
Due to a large surface area, small, hollow, and layered
structures, carbon nanotubes (CNTs) have already been inves-
tigated as promising adsorbents for various organic pollutants
and metal ions and can be easily modified by chemical treat-
ment to increase their adsorption capacity (Chen et al., 2009b).
CNTs have been used for the treatment of heavy metals
contaminated aqueous solutions. Unlike many adsorbents,
CNTs possess different features that contribute to the superior
removal capacities; such as fibrous shape with high aspect ratio,
large accessible external surface area, and well developed
mesopores. The pores have been reported to be mostly meso-
pores due to a high van der Waals interaction forces along the
length axis (Wang et al., 2006; Inoue et al., 1998; Girifalco et al.,
2000). The uses of CNTs as support of metallic oxides have
still been reported (Xie and Gao, 2007; Takenaka et al., 2008). The
materials have the advantages of high sorption capacity, large
surface area and supported metallic oxides. Chemical oxidation
polymerization, followed by the carbonization process has been
employed to produce iron oxide-impregnated magnetic CNT
composites. A solvo-thermal method has been also used to
synthesize CNTeiron oxide composites. Other effective
approaches, including the arc-discharge technique and elec-
trolysis deposition, to prepare CNT-based functional materials
have been developed (Zhenyu et al., 2005). The adsorption
behavior of carbon nanotubeeiron oxides magnetic composite
has been investigated for the removal of Pb(II) and Cu(II) from
water (Peng et al., 2005), Ni(II) and Sr(II) (Chen et al., 2009a) and
cationic dyes (Gong et al., 2009).
The application of magnetic particle technology to solve
environmental problems has received considerable attention
in recent years. For this, the objective of this study was to
prepare and characterize carbon nanotube/nano-iron oxide
composites and to demonstrate how it could be utilized for the
removal of chromium (III) in such simple batch mode and
subsequent fixed bed treatment methods.
2. Experimental
2.1. Materials
Nitric acid, chromium nitrate and ferric and ferrous chlorides
were all obtained from SigmaeAldrich. Chromium 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.
Activated carbon (Darco G-60) was from Fisher Scientific
Company. All other chemicals were of analytical grade. Stock
solutions were prepared daily by dissolving in distilled water.
2.2. Synthesis of MWCNTs/nano-iron oxide
The multiwall carbon nanotubes (MWCNTs) used in this study
as a building block, were of more than 95% purity and procured
commercially. MWCNTs was of the following specifications;
purity, >95%; outer diameter, 30e50 nm; inside diameter,
5e10 nm; 30e50 nm; length, 10e20 mm. The purification
process using HNO3 was performed to remove impurities if any
and to modify the surface of the tube with carbonyl and
hydroxyl groups. The purification process was accomplished
by stirring MWCNTs in concentrated nitric acid at 70  C for 12 h,
followed by filtering and washing with distilled water, and then
drying at 110  C for 6 h. Then, MWCNTs were oxidized by
refluxing with 50% nitric acid at 120  C for 12 h under stirring
conditions. The product was then filtered and rinsed with
doubly distilled water and dried overnight in the oven.
The preparation of MWCNTs/nano-iron oxide composites
was accomplished as follows. All glassware was cleaned by
aqua regia freshly prepared prior to use. A mixed solution of
0.1 M ferric chloride hexahydrate and 0.05 M ferrous chloride
tetrahydrate with a molar ratio of one to two was prepared.
Subsequently, a specific amount of oxidized MWCNTs was
suspended in the mixed solution for 2 h. Then, at constant
temperature of 70  C, 5 M- NH4OH solution was added drop
wise to precipitate iron oxides. The mixture was adjusted to
pH 10 and then aged for 1 h under stirring. After the comple-
tion of the reaction, the suspension was allowed to cool. The
product was separated by magnet then washed by distilled
water and ethanol respectively. The obtained composite was
dried in an oven at 100  C for 2 h.
2.3. Characterization methods
The size and morphology of the magnetic composites were
characterized by scan electron microscopy (SEM) using a field
emission scanning electron microscope (FESEM, FEI Nova-
Nano SEM-600, Netherlands). The structure phases and
average size of the synthesized adsorbents was analyzed by
X-ray diffraction (XRD) (Shimadzu XRD Model 6000). Infrared
absorption spectroscopy (IR) spectra were measured at room
temperature on a Fourier transform infrared (FTIR) spectros-
copy using the KBr Pellet technique.
2.4. Adsorption experiments
2.4.1. Batch adsorption experiments
Batch adsorption experiments were conducted by adding the
composite mass to 50 mL of different Cr(III) test solutions at
different pH (3e7) in an Erlenmeyer flask (100 mL capacity). The
initial solution pH was adjusted using 0.1 M HCl or 0.1 M NaOH.
The flasks were agitated at different speed (0-to-150 rpm) in
a rotary shaker for different contact time (10e60 min). The
composite mass was separated from the test solution by magnet
followed by filtration using a vacuum filter. For the fixed bed
system, the column surrounded with a magnet was packed with
the synthesized composites. Then the prepared Cr(III) solutions
were passed through to study the adsorption capacity. The
column diameter and length used in every experiment were
kept constant with a bed depth of 1 cm and diameter of 0.3 mm.
The different layer thickness of the adsorbent and the flow rate
of the solutions were used as specified for each experiment.
All experiments were carried out at ambient temperature
(25  2  C). The amount of chromium adsorbed was calculated
from the difference between its concentration in test solution
and in the supernatant liquid. The initial and final concen-
trations of chromium were analyzed by using inductively
 w a t e r r e s e a r c h 4 5 ( 2 0 1 1 ) 2 2 0 7 e2 2 1 2
Fig. 1 e SEM images of (A) oxidized MWCNTs (B) MWCNTs/nano-iron oxide.
coupled plasma mass spectrometry (ICP-MS). The samples
were filtered prior to spray chamber applications to remove
the possible agglomerates.
3. Results and discussion
3.1. Characterization of MWCNT/nano-iron oxide
After the synthesis of MWCNT/nano-iron oxide composite,
a test with the magnet showed that the whole material is
magnetic and completely attracted to the magnet. The
morphologies of uncoated MWCNTs and synthesized MWCNT/
nano-iron oxide were obtained by SEM. Fig. 1A and B shows the
SEM images of oxidized MWCNTs and the composites, respec-
tively. SEM image (Fig. 1B) of the composites depicts an entan-
gled network of oxidized MWCNTs with clusters of iron oxides
Fig. 2 e X-ray diffraction of (A) oxidized MWCNTs (B)
MWCNTs/nano-iron oxide where Mn: Magnetite (Fe3O4);
Mh: Maghemite (g-Fe2O3).
2209
attached to them. Surface area of the prepared composite was
measured using BET method. The specific surface area of
MWCNT/nano-iron oxide composite was 92 m2/g.
Under the reaction conditions employed, four iron oxides
are commonly formed. These are Fe3O4 (magnetite), g- Fe2O3
(maghemite), a-Fe2O3 (hematite) and a-FeO(OH) (goethite).
Among them two magnetite and maghemite are magnetic
(Perez et al., 1998). Fig. 2A and B shows the X-ray diffraction
patterns of MWCNTs and MWCNTs/nano-iron oxide compos-
ites. The two peaks corresponding to the structure of MWCNTs
also exist in the XRD pattern of the magnetite composites. The
XRD pattern of the magnetic composites reveals a cubic iron
oxide phase. The presence of maghemite and magnetite as the
magnetic phase in the composite is supported by their indexes
diffraction peaks as shown in Fig. 2B. The average grain size ‘d’
of the iron oxide was estimated by using the standard equation
known as Debye Scherrer formula (Yu et al., 2009).
0:9l
d¼
bcosq
where l ¼ wavelength of the X-ray, b ¼ FWHM (Full Width at
Half Maximum) width of the diffraction peak, q ¼ diffraction
angle. The average size of iron oxide was 18 nm.
Fig. 3 e FTIR spectra of (A) oxidized MWCNTs (B) MWCNTs/
nano-iron oxide.
2210 w a t e r r e s e a r c h 4 5 ( 2 0 1 1 ) 2 2 0 7 e2 2 1 2

FTIR measurements are used in order to confirm the

formation of iron oxide. FTIR spectra, Fig. 3A and B of oxidized
MWCNTs and synthesize MWCNTs/nano-iron oxide were
performed for a better comprehension of the structure and
composition of these materials. An absorption band revealing
the vibrational properties of FeeO bond is observed for in
around 477 cm1. This band is mainly assigned to the
stretching vibrations of FeO (yFeO). The broad absorption
peaks in the range of 3300e3500 cm1 correspond to eOH
group, indicating existence of the hydroxyl groups on the
surface of the composites or it can be attributed to the
adsorption of some atmospheric water during FTIR measure-
ments. Those at 1570e1655 cm1 are the C]O stretching
mode of the functional groups on the surface of the MWCNTs.
The two peaks at 2920 and 2854 cm1 correspond to the CeH
stretch vibration, originated from the surface of tubes, Fig. 3A, Fig. 5 e The effect of pH on the amount of Cr(III) adsorbed
are obviously weak in Fig. 3B. on the MWCNT/nano-iron oxide (Conditions: as in Fig. 4).

3.2. Results of batch experiments

surface of MWCNTs which are also available for electrostatic

3.2.1. Effect of contact time
interaction with the chromium. It should be noticed that in
The influence of contact time on the adsorption capacity of
the composite there are two sorts of adsorbing sites; MWCNTs
activated carbon, MWCNTs and the produced composite is
and iron oxide nanoparticles.
depicted in Fig. 4. Less than 5% adsorption by activated carbon
was observed. According to the literature reports activated
3.2.2. Effect of pH
carbon is expected to have a poor adsorption capacity for
The pH effect on the adsorption of Cr(III) onto the prepared
removal of contaminants comparing with MWCNTs. It is
composite was studied by evaluating the adsorption at pH
clearly stated that one of the disadvantages of using activated
values of 3, 4, 5, 6, and 7 as shown in Fig. 5. It was found that
carbon is that it presents problems with the adsorption of
the composite effective for the adsorption of Cr(III) above pH 3
hydrophilic substances (Kandah and Meunier, 2007; Pillay
and below pH 7, since Cr(III) at strongly acidic media did not
et al., 2009). Both MWCNTs and the MWCNTs/nano-iron
adsorb to the composite. Fig. 5 illustrates that maximum
oxide by contrast, show a good ability to remove Cr(III) from
adsorption capacity at pH 5e6.
aqueous solution. The MWCNTs/nano-iron oxide, however,
The result could be explained based on the reported
show a greater ability, approximately 90% adsorption after
speciation diagrams (Zhang et al., 2008; Richard and Bourg,
60 min contact time. This can be explained by the additional
1991; Chuan and Liu, 1996). It has been reported that at pH
adsorbing sites that provided by the oxygen atoms of iron
less than 3.6, Cr(III) is present as Cr3þ while at pH higher than 4
oxide nanoparticles, average size is 18 nm, Fig. 2B, on the
and lower than 6.5, it is present as Cr(OH)2þ Cr(OH)þ 2 . However,
it is present as neutral Cr(OH)3 species at pH between 7 and 12.
On the other hand, the point of zero charge (PZC) of
oxidized MWCNTs was reported to be approximately 4 (Lu and
Chiu, 2006; Gao et al., 2009). Thus, when it is placed in aqueous

Fig. 4 e The effect of contact time on the amount of Cr(III)

adsorbed on different adsorbents (Conditions: initial
Chromium concentration 20 ppm; Dosage of Fig. 6 e The effect of agitation speed on the amount of
adsorbent [ 50 mg; pH 6; Agitation speed [ 150 rpm). Cr(III) adsorbed on the MWCNT/nano-iron oxide.
 w a t e r r e s e a r c h 4 5 ( 2 0 1 1 ) 2 2 0 7 e2 2 1 2
Fig. 7 e The effect of dosage on the amount of Cr(III)
adsorbed on the MWCNT/nano-iron oxide.
solutions of pH below its PZC ¼ 4 it becomes protonated and
exhibits a positive net charge on its surface, thus it could not
well adsorb the Cr3þ. In contrast, when placed in solutions
above its PZC ¼ 4, the net surface charge turns negative by
deprotonation and it could adsorbs the positively charged
chromium species. At pH 7, the chromium presents as neutral
Cr(OH)3 species which has low affinity for electrostatic inter-
action with the positively charged composite of MWCNTs.
Therefore, at pH 7, columbic or electrostatic interactions do
not favor the adsorption of chromium. The maximum Cr(III)
removal was 82 and 88% at pH 5 and 6, respectively. The
association between Cr(III) and the composite is therefore
governed by Cr(OH)2þ species, since Cr(OH)2þ dominates the
system within this pH range (Richard and Bourg, 1991; Chuan
and Liu, 1996).
3.2.3. Effect of agitation speed
The effect of agitation speeds was investigated by a range from
0 rpm to 150 rpm, Fig. 6. The adsorption of Cr(III) was low
without or at low agitation speed and rose as the agitation
speed was increased to 150 rpm. This effect can be attributed to
the decrease in boundary layer thickness around the adsorbent
particles being a result of increasing the degree of mixing.
Fig. 8 e The effect of flow rate (mL/min) on the amount of
Cr(III) adsorbed on the MWCNT/nano-iron oxide.
2211
Fig. 9 e The effect of layer thickness on the amount of
Cr(III) adsorbed on the MWCNT/nano-iron oxide.
3.2.4. Effect of dosage of adsorbent
Various amounts of adsorbent ranging from 5 mg to 100 mg
were used. The percentage removal of Chromium ions varied
linearly with the amount of the adsorbent as shown in Fig. 7.
3.3. Results of fixed bed experiments
3.3.1. Effect of flow rate
Experiments were performed with flow rates of 1e5 mL/min
whereas the thickness of the adsorbent was 3 mm. As depic-
ted in Fig. 8, it was observed that the lower the flow rate the
higher the chromium removal. This is due to the more contact
time when the flow rate is low.
3.3.2. Effect of bed thickness
The removal of Cr(III) by MWCNTs/nano-iron oxide fixed bed
composite of different thickness at a constant flow rate of
1 mL/min. As shown in Fig. 9, by increasing the thickness of
the fixed bed layer, the uptake of chromium ions increases.
Increasing the fixed bed layer leads to increase of the available
interaction sites of the composite that provided more sites for
adsorption of chromium ions with a thicker layer and the
efficiency is increased by allowing sufficient time for the
adsorbate to diffuse into the adsorbent.
When the thickness of the layer of the composite was
increased from 0.5 mm to 3 mm, the percentage removal was
increased from 40% to 90%. Comparing with its efficiency in
batch mode, the prepared adsorbent displayed the main
advantage of separation convenience when a fixed bed
column was used. This is because the chromium anions are
forced to interact with the active adsorbing sites on the large
surface-area composite during the penetration.
4. Conclusion
The MWCNT/nano-iron oxide magnetic composites were
prepared. Characterization using XRD suggests that the
magnetic phase formed is maghemite and magnetite. SEM
image shows clusters of nano-iron oxides attached to a network
2212 w a t e r r e s e a r c h 4 5 ( 2 0 1 1 ) 2 2 0 7 e2 2 1 2
of MWCNTs. The adsorbents show good adsorption capacity for
chromium ions. The adsorption capability of the composite is
higher than that of MWCNTs and activated carbon. In the batch
mode, it was found that the adsorption capability is increased
by increasing the agitation speed and it is pH dependent. The
experiments performed in the fixed bed mode revealed that the
removal capability of the composites for chromium increases
with decreasing the flow rate. Our results demonstrate that the
MWCNTs/nano-iron oxide magnetic composites, whose
surface area is large, are very promising materials as adsorbent
for contaminants in water with good performances. The
material reported here could be used as a base for encapsulation
in reverse osmoses systems. We believe it is required to have
a small material with large surface area and good ability to
remove pollutants, especially for compact columns used in
water filtration units.
Acknowledgement
Tawfik A. Saleh acknowledges the support of King Fahd
University of Petroleum and Minerals, (KFUPM) Dhahran,
Saudi Arabia for this work.
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