Journal of Environmental Management 90 (2009) 3340–3344

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Journal of Environmental Management

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

Evaluation of a low-cost adsorbent for removal of toxic metal ions

from wastewater of an electroplating factory
Francisco W. Sousa a, Marcelo James Sousa a,1, Isadora R.N. Oliveira a,
André G. Oliveira a, Rivelino M. Cavalcante a, Pierre B.A. Fechine a,
Vicente O.S. Neto b, Denis de Keukeleire c, Ronaldo F. Nascimento a, *
a
Laboratório de Análise Traço, Departamento de Quı́mica Analı́tica e Fı́sico Quı́mica, Universidade Federal do Ceará, Campus do Pici, Centro de Ciências,
Bloco 940-CEP: 60451-970 Fortaleza, Ceará, Brazil
b
Universidade Estadual do Ceará, Centro de Ciências e Tecnologia. Av. Paranjana, 1700 Campus do Itaperi, 60740-000 Fortaleza, CE – Brazil
c
Ghent University, Faculty of Pharmaceutical Sciences, Harelbekestraat 72, 9000 Ghent, Belgium

a r t i c l e i n f o a b s t r a c t

Article history: In this study, sugar cane residue or bagasse was used for removal of toxic metal ions from wastewater of
Received 15 August 2008 an electroplating factory located in northeast Brazil. Prior acid treatment increased the adsorption
Received in revised form efficacies in batch wise experiments. The microstructure of the material before and after the treatment
6 April 2009
was investigated by X-ray diffraction, infrared spectroscopy and scanning electron microscopy. Column
Accepted 7 May 2009
Available online 17 June 2009
operations showed that removals of Cu2þ, Ni2þ and Zn2þ from wastewater (in the absence of cyanide)
were 95.5%, 96.3.0%, and 97.1%, respectively. Regeneration of the adsorbent obtained in acid indicated
that the efficiencies decreased only after the fourth cycle of re-use. Acid-treated sugar cane bagasse can
Keywords:
Electroplating wastewater be considered a viable alternative to common methods to remove toxic metal ions from aqueous
Toxic metal ions effluents of electroplating industries.
Adsorption Ó 2009 Elsevier Ltd. All rights reserved.
Sugar cane bagasse

1. Introduction
It is well known that metal salts cause environmental pollution
and that their discharge in wastewater can have adverse effects for
life on earth. Stringent control is, therefore, mandatory (McKay,
1995; Atkinson et al., 1998). However, the absence of an environ-
mental policy and strict laws in combination with a lack of
investments to treat toxic wastewaters from small and medium-
size electroplating industries have led to uncontrolled discharges of
effluents in the environment. Such wastewaters often contain
cyanide complexes with metals including copper, nickel, zinc, etc.,
which should be removed prior to discharge (Atkinson et al., 1998).
In this context, the city of Juazeiro do Norte (236,000 inhabi-
tants), located in Ceará, Brazil, has about 100 electroplating facto-
ries (registered and unregistered) and most of these do not have an
efficient treatment system for their wastewaters. Analysis has
* Corresponding author. Tel.: þ55 85 3366 9958; fax: þ55 85 3366 9982.
E-mail address: ronaldo@ufc.br (R.F. Nascimento).
1
in memoriam.
revealed high levels of Ni2þ, Cu2þ, Zn2þ and CN (Barros et al.,
2008). Taking into account that water resources in this area are very
valuable for regional development, cleaning is mandatory.
Metals are commonly removed from effluents by precipitation,
ion exchange methods, and electrolytic techniques. Adsorption on
activated carbon has been investigated intensively (McKay, 1995;
Cooney, 1999), although the high cost for recycling is a drawback for
developing countries (Pollard et al., 1992). The applicability of
biomass (Kapoor and Viraraghavan, 1995; Holan and Volesky, 1995;
Sandau et al., 1996; Wase and Forster, 1997; Aksu, 2001; Horsfall
et al., 2003; Salim et al., 2008) and agricultural residues as low-cost
adsorbents (McKay, 1995; Bailey et al., 1999; Amarasinghe and
Williams, 2007; Aydin et al., 2008; Gupta et al., 2009; Sawalha et al.,
2009; Sousa et al., 2008; Wang et al., 2009) has received great
attention. There is a growing interest in using cheap agricultural
by-products, such as residues of sugar cane and coconut fiber
(Amarasinghe and Williams, 2007; Sousa et al., 2008).
This work aims at developing a simple laboratory-scale
adsorption procedure to treat wastewaters derived from electro-
plating factories using sugar cane bagasse that is abundantly
available in the region of Juazeiro do Norte.

0301-4797/$ – see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jenvman.2009.05.016
 F.W. Sousa et al. / Journal of Environmental Management 90 (2009) 3340–3344
2. Materials and methods
2.1. Chemicals and reagents
Sugar cane bagasse was provided from a sugar cane spirit
factory (Fortaleza, Brazil). Standard solutions of metal ions
(1000 mg L1), composed of Cu(NO3)2.6H2O, Zn(NO3)2.6H2O, and
Ni(NO3)2.6H2O were purchased from Merck (São Paulo, Brazil). HCl,
HNO3, and H2SO4 were of analytical grade (VETEC, São Paulo,
Brazil). The concentrations of ions were determined by atomic
absorption spectrophotometry (AAS, GBC 933 plus model) in an air-
acetylene f1ame.
2.2. Adsorbent preparation
Sugar cane bagasse (20–48 mesh) was first treated with acid
(1.0 mol L1 HCl and HNO3) for 24 h, washed with de-ionized water,
and dried at room temperature. The adsorbent was then stored in
sealed flasks in a vacuum desiccator before use.
2.3. Column adsorption
Column adsorption experiments were carried out using a poly-
ethylene column (30 cm  1.5 cm I.D) packed with 4.0 g treated
sugar cane bagasse. Removal efficiencies were obtained using
wastewater from electroplating factories in Juazeiro do Norte.
Breakthrough curves were used to investigate the column capac-
ities at complete exhaustion. Thus, 200 mL of wastewater were
percolated using a peristaltic pump at a flow rate of 2.0 mL/min and
breakthrough curves were obtained by plotting C/Co versus volume
collected (10 mL) at the exit of the column. Adsorbent regeneration
and metal recoveries were studied in acid (2.0 mol L1 HCl). Metal
desorption was achieved by washing the column with distilled
water followed by 5 aliquots of 10 mL (2.0 mol L1 HCl) and rinsing
with de-ionized water for re-use.
2.4. Structural characterization of the sugar cane bagasse
The main functional groups present in sugar cane bagasse
(treated and untreated) were characterized by infrared spectros-
copy using a FTLA 2000-102, ABB-BOMEM apparatus.
Surface morphology and microstructure were studied by scan-
ning electron microscopy (SEM) using a model DSM 960/Zeiss, with
a 20 kV electron beam. The sample was coated with gold (sputter
couter) in argon plasma (model BAL.ZERS 5CD50).
X-ray diffraction (XRD) patterns were obtained at room
temperature (300 K) by step scanning using a diffractometer
Rigaku, model DMAXB. The samples were pulverized and the
particles were compacted in a cylindrical mold into disc format (Ø
1.7 cm) and pressurized at 111 MPa. There were five seconds of
counting time for each step, with a Cu-Ka tube at 40 kV and 25 mA,
using the Bragg – Bretano geometry in continuous mode with
a speed of 0.5  /min and a step size of 0.02 (2q) in the angular
range 5–35 (2q). The sugar cane bagasse crystal line fraction (F)
was obtained through separation and integration of crystal line and
amorphous peak areas under the diffraction X-rays plots, using
Equation (1):
P Ion
IC
F ¼ P
ðIC þ IA Þ
where: IC is the diffractogram total crystalline phase area, IA is the
diffractogram total amorphous phase area.
3341
3. Results and discussion
3.1. Treatment of adsorbent material
The adsorption efficiencies of the untreated and the acid-treated
sugar cane bagasses have been previously investigated by batch
adsorption with a mixture of metal ions (100 mg L1 at pH 5.0). The
results are shown in Table 1. It can be observed that the adsorption
capacity of the acid-treated material is superior to that obtained for
the untreated material. This can be due to adsorption of metal
complexes formed in the presence of cyanide. Considering our
results, treatment with 1.0 M HCl was used as a basis for further
studies. Physical properties: particle size: 0.833–0.317 mm, packing
density: 0.075 g/mL, bulk density: 0.051 g/mL: bed porosity:
13.32%.
3.2. Microstructure of the sugar cane bagasse
Fig. 1 shows the XRD patterns of the untreated (a) and acid-
treated (b) sugar cane bagasses. There are two main peaks repre-
senting planes 002 and 101 with directions on 22.24 and 16.2 ,
respectively. They are characteristic of the cellulose crystalline
phase. In addition, a large amount of amorphous lignin could be
detected. When its concentration increases, the crystal line fraction
(F) decreases. The F value for the untreated material (0.62) was
close to the acid-treated material (0.67). We also observed three
other peaks on 26.52 , 29.36 and 30.84 for both samples that
could be attributed to impurities such as SiO2 and CaCO3, whose
intensities decreased after acid treatment (Fig. 1 (b)).
The functional groups present in sugar cane bagasse can be
determined by infrared spectroscopy (IR) (Fig. 2 (a) and Fig. 2 (b)).
Since sugar cane bagasse contains 30–50% cellulose and 20–24%
lignin (Pandey et al., 2000; Vieira et al., 2007), their main absorp-
tions are evident in IR, as has been shown by Bilba and Ouensanga
(1996). We observed that acid treatment removed or decreased
some modes of lignin: absorptions due to C–Hn (alkyl and aromatic)
stretching vibrations (2918 and 2850 cm1), absorptions charac-
teristic of the C]O stretching vibration (1708 cm1), and a signal
typical of an aromatic skeleton (1604 cm1). It can also be noted
that the intensities of almost all bands were lower after acid
treatment.
To obtain more information on the microstructure of our
materials, SEM micrographs were obtained at an amplification of
20 (Fig. 3 (a) and Fig. 3 (b), respectively). The untreated sugar cane
bagasse had a reasonable homogeneity (aggregate shape) (Fig. 3
(a)). However, after acid treatment, the sample presented fibrous
and flake shapes (Fig. 3 (b)) due to the globular shape formed with
cellulose and lignin fibers could be observed at an amplification of
1000 (Fig. 3 (c)), since the chemical treatment assisted dispersion
of the fibers, i.e., improved the contact area.
3.3. Breakthrough curves
According to the literature (Patil and Paknikar, 1999; Bose et al.,
2002), aqueous solutions containing high copper concentrations
Table 1
Comparison of the adsorption efficiencies of toxic metal ions on untreated and acid-
treated sugar cane bagasse.
Q (mg metal/g adsorbent)
Acid-treated Acid-treated Untreated
(1) (1.0 mol L1 HCl) (1.0 mol L1HNO3)
Cu2þ 0.217 0.211 0.050
Ni2þ 0.135 0.228 0.063
Zn2þ 0.176 0.120 0.0137
3342 F.W. Sousa et al. / Journal of Environmental Management 90 (2009) 3340–3344

a
Intensivity (a.u)

5 10 15 20 25 30 35
2θ (degree)

Fig. 1. X- ray diffractogram of (a) untreated and (b) acid-treated sugar cane bagasse.

and relatively low concentrations of zinc, nickel and cyanide (at

pH < 2), contain weak complexes of nickel and zinc in negligible
concentrations. In contrast, copper-cyanide is present in appre-
ciable quantities due to high affinity of copper for cyanide (Bose
et al., 2002) Breakthrough curves were investigated in the
untreated effluent containing copper, nickel, zinc, and cyanide ions
at pH 1.26. Next, a sample was treated by alkaline chlorination for
cyanide destruction. The method involved overnight treatment
with 2.0 mol L1 NaOCl for total oxidation of cyanide to inorganic
carbon (Yalçin et al., 2000). The precipitate was dissolved in
1.0 mol L1 H2SO4 to yield a final solution with metal concentra-
tions of 200 mg L1, 14.4 mg L1, and 65.5 mg L1 of Cu2þ, Ni2þ and
Zn2þions, respectively. 200 mL of the solution was percolated
through a column (4.0 g adsorbent) at a flow rate of 2.0 mL min1
and 10 mL eluted volume was collected to obtain the breakthrough
curves presented in Fig. 4(a) and (b). It can be seen that the column
capacity at complete exhaustion reached a plateau when the
effluent volume was about 70.0 mL.
Percentage for removal of the toxic metal ions was determined
from breakthrough curves (Table 2). It was observed that removal

Fig. 3. SEM (Scanning Electron Microscopy) of untreated sugar cane bagasse (a) before
and (b) after acid treatment (amplification of 20), and (c) globular shapes (amplifi-
a cation of 1000).
Transmitance (a.u.)

of all ions was enhanced in the absence of cyanide. However, in the

presence of cyanide, a considerable reduction in removal of zinc
(67.0%) and nickel (65.5%) ions was noted, while removal of copper
(91.2%) ions was not much affected (Table 2).
The increase on removal of copper-cyanide complexes in acidic
conditions may be due to the formation from insoluble specie CuCN
(Patil and Paknikar, 1999; Bose et al., 2002).
b The results revealed a contrast for zinc and nickel ions, which
form relatively complexes with cyanide in aqueous solutions that
are much weaker than copper cyanide complexes (Bose et al.,
4000 3500 3000 2500 2000 1500 1000 500 2002). These metals predominantly exist in uncomplexed form in
Wavenumber (cm-1) the presence of cyanide. Thus, a considerable decrease in adsorp-
tion of zinc and nickel ions on the sugar cane bagasse surface (at pH
Fig. 2. Infrared spectra of (a) untreated and (b) acid-treated sugar cane bagasse. 1.26) is expected, which is probably due to electrostatic repulsion
 F.W. Sousa et al. / Journal of Environmental Management 90 (2009) 3340–3344 3343

a 1,2
Cu Cu(II)
Ni 200 Ni(II)
1,0 Zn(II)
Zn

0,8

Amount adsorbed (mg/L)

150
C/Co

0,6

0,4
100
0,2

0,0
0 10 20 30 40 50 60 70 80 90 100 110 50
Vol, ml

1,4
b
Cu
1,2 Ni 0
Zn 0 20 40 60 80 100
1,0 Volume of eluent (mL)

Fig. 5. Desorption of toxic metal ions with 2.0 mol L1 HCl using sugar cane bagasse.
0,8
C/Co

This procedure was repeated 5-times with the same adsorbent in

0,6
the column. The results, shown on Fig. 6, indicated that the removal
efficiency decreased to 79.6% for Cu2þ, 77.4% for Zn2þ, and 73.8% for
0,4
Ni2þ during the first and the fourth cycles. However, a considerable
efficiency decrease was observed after 4 cycles due to depletion of
0,2
binding sites caused by the acidic elution (Gupta et al., 2009).

0,0
0 10 20 30 40 50 60 70 80 90 100 110 3.5. Comparison with conventional adsorbents
Vol, ml
A comparison of removal capacities of metal ions by low-cost
Fig. 4. Breakthrough curves of toxic metal ions: (a) wastewater with cyanide (18 mg/L) sugar cane bagasse with other adsorbents is provided in Table 3.
and (b) wastewater after NaOCl oxidation of cyanide. Amount of adsorbent: 4.0 g,
Cu2þ: concentration: 200 mg/L at pH 1.78 and flow rate of 2.0 mL/min. C/Co represents
the ion concentrations for initial and final solutions.
100

between the cationic sugar cane bagasse surface and the zinc and 100,5
nickel cations.
95
Amount removal (%)

100,0
3.4. Column regeneration
Amount removal (%)

Column regeneration was carried out by elution with acid under 90 99,5

conditions used for the breakthrough curves. The results shown on

Fig. 5 indicate that 50 mL of acid eluent is efficient for desorption of
99,0
the retained metals. The first aliquot of 30 mL eluted more than 50% 1 2 3 4 5

of adsorbed ions, while the remaining eluent volume of 20 mL led 85 Cycle number

to complete desorption.
Recycling of the column was evaluated by passing 30 mL water
through the column, followed by 60 mL of the sample solution as 80
such and 70 mL 2.0 mol L1 HCl for elution of retained metal ions.
Cu (II)
Table 2 Ni (II)
75 Zn (II)
Percentages of removal of toxic metal ions from wastewater of an electroplating
factory using sugar cane bagasse (obtained from Fig. 4 (a) and (b)). Conditions: pH
1.26; flow: 2.0 mL/min; mass of the adsorbent: 4.0 g; temperature: 28  2  C. 1 2 3 4 5
Wastewater Cu 2þ
(200 mg/L) 2þ
Ni (14.4 mg/L) Zn2þ
(65.5 mg/L) Cycle number
With cyanide (18.1 mg/L) 91.2% 65.5% 67%
Fig. 6. Removal efficiencies of toxic metal ions from wastewater of an electroplating
After removal of cyanide 95.5% 96.3% 97.1%
factory and number of cycles using sugar cane bagasse.
3344 F.W. Sousa et al. / Journal of Environmental Management 90 (2009) 3340–3344

Table 3
Comparison of the adsorption efficiencies of toxic metal ions on acid-treated sugar cane bagasse with other adsorbents.

Adsorbent Cu2þ (mg/g) Ni2þ (mg/g) Zn2þ (mg/g) pH Flow rate (mL/min) Mass of adsorbent (g) Reference
Sugar cane bagasse 4.08 0.29 0.90 1.26 2.0 4.0 This work
Coconut Shell 10.13 3.66 1.56 5.0 2.0 0.4 Sousa et al., 2008
Tea waste 48 – – 5–6 20 15.0 Amarasinghe and Williams, 2007
Activated carbon 38.0 9.9 – – 2.0 3.0 Monser and Adhoum, 2002
Biomass 2.89 – 1.08 5–7 3.0 4.7 Kapoor and Viraraghavan, 1998
Zeolite 0.125 – – 5.0 5.4 15.0 Han et al., 2006

Activated carbon (Monser and Adhoum, 2002) proved to be supe-
rior, but acid-treated sugar cane bagasse was more efficient in
removal of metal ions than biomass (Kapoor and Viraraghavan,
1998) and performed even better than zeolite (Han et al., 2006).
4. Conclusion
Structural characterization of sugar cane bagasse showed clear
differences before and after acid treatment, which has improved
the purity of the material and increased the contact area.
The percentages of removal of the ions from wastewater of an
electroplating factory were 95.5% for Cu2þ, 97.3% for Zn2þ, and
96.3% for Ni2þ ions using acid-treated sugar cane bagasse. The
adsorbent could be recycled in acidic conditions while the feasi-
bility of re-use was observed after 4 cycles. It can be concluded that
acid-treated sugar cane bagasse can be considered a low-cost
alternative for removal of toxic metal ions from aqueous industrial
effluents.
Acknowledgements
The authors thank the Brazilian agencies CNPq and FUNCAP for
financial support of and the Federal University of Ceará (Depart-
ment of Analytical Chemistry and Physical Chemistry) and PADE-
TEC for the use of their facilities. We also thank Prof. Vicente
Oliveira Sousa Neto (Universidade Estadual do Ceará) for revision of
the manuscript.
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