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Article history: In this study, the adsorption of lead (Pb2þ) onto activated carbon (AC) originating from cow bone,
Received 15 February 2013 chemically modified with HNO3, was investigated. Physico-chemical carbon characterization assays and
Received in revised form the determination of the optimum pH conditions and contact time, as well as studies on the kinetic and
7 August 2013
isothermal equilibrium and adsorbent reuse, were carried out. The AC presented a greater amount of acid
Accepted 10 August 2013
Available online xxx
functional groups than basic groups at the surface, making it efficient for cationic exchange. The pHPZC
was 4.0 and the minimum contact time required for the assays to be performed was 6 h. It was observed
that the time required to reach kinetic equilibrium decreased with increasing initial metal concentration
Keywords:
Metal removal
in solution and the values found for qexp were 32.1, 50.1 and 42.3 mg g1 for concentrations of 100, 150
Environmental technology and 200 mg L1, respectively. The pseudo-second-order kinetic model best represented the experimental
Adsorption data for all initial lead concentrations studied, presenting good linear correlation coefficients. The
Lead Langmuir and Freundlich models were used to fit the experimental data and these showed good cor-
Activated carbon relations, with the Langmuir model providing a better description of the equilibrium (higher R2 value). It
was verified that the HCl desorption showed the highest efficiency; the minimum time to reach the
desorption equilibrium was 3 h and the recovery was approximately 50%. The proposed adsorption
process efficiently removes lead present in aqueous solution and can be used in industrial processes.
Ó 2013 Elsevier Ltd. All rights reserved.
1. Introduction resource is associated with shortages that are partly due to the
accumulated contamination of water resources over years of in-
The need for the use of water in virtually all human activities, dustrial exploitation. In recent years, the environmental organs
whether urban, rural or industrial in nature, is undeniable. How- concerned with the quality of the environment have established
ever, despite being of crucial important for human survival, this stricter environmental laws for the disposal of effluents, causing
the chemical industry to increase investment in research with a
focus on the treatment of its liquid effluents and solid wastes.
Abbreviations: Ce, concentration of adsorbate in solution at equilibrium Among the contaminants present in industrial waste, heavy
(mg L1); kF, Freundlich constant for adsorption capacity of the adsorbent (L g1); metals receive considerable attention from scientists and engineers
kL, constant for the Langmuir adsorption equilibrium (L mg1); k1, constant of the
pseudo-first-order kinetics model (min1); k2, constant of the pseudo-second-order
due to their toxic nature and the adverse effects of metals on the
kinetics model (g mg1 min1); m, mass of activated carbon (g); n, Freundlich receiving water bodies. Unlike most organic pollutants, heavy
constant for the adsorption intensity (adim.); qe, amount of metal ions adsorbed at metals are usually refractory and are not easily degraded (Sekar
equilibrium (mg g1); qexp, amount of ions adsorbed experimentally (mg g1); qm, et al., 2004). As heavy metals are not decomposed into non-toxic
effective adsorption capacity (mg g1); qt, amount of metal ions adsorbed at
end products, their concentrations should be reduced to accept-
different times (mg g1); q1, amount of metal ions adsorbed at equilibrium e
pseudo-first-order kinetics (mg g1); q2, amount of metal ions adsorbed at equi- able levels before disposal into the environment (Sulaymon et al.,
librium e pseudo-second-order kinetics (mg g1); RL, Langmuir equilibrium 2009).
parameter (adim.); R2, linear correlation coefficient (adim.); t, adsorption time (min The lead present in the wastewater of many industrial processes,
or h). such as the production of paint coatings, dyes, glass and batteries
* Corresponding author. Tel.: þ55 48 3721 5231.
E-mail addresses: maria.cechinel@posgrad.ufsc.br, maria.alice.cechinel@
(Li et al., 2010), is potentially toxic to humans and to the aquatic
hotmail.com (M.A.P. Cechinel), selene@enq.ufsc.br (S.M.ArrudaG. Ulson de Souza), environment. The main consequences in the environment are the
augusto@enq.ufsc.br (A.A. Ulson de Souza). poisoning of aquatic organisms and severe changes in the aquatic
0959-6526/$ e see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jclepro.2013.08.020
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
2 M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8
fauna and flora. For humans, constant exposure to lead causes preparation requires long processing steps. Al-Asheh et al. (2003)
edema, learning disabilities in children, damage to organs such as have presented results obtained for the adsorption of metals us-
the liver, kidneys and heart, and immune system disorders ing chicken feathers.
(Sreejalekshmi et al., 2009). The maximum lead discharge into Activated carbon originating from cow bone is traditionally used
receiving bodies allowed by Brazilian legislation (CONAMA, 2005) industrially to remove color from sugar (Moreno-Piraján et al.,
is 0.5 mg L1 and the current limit according to the USEPA for 2010), but its adsorbent characteristic has stimulated its use in
drinking water is 0.015 mg L1 (Momcilovic et al., 2011). several other areas, including the removal of metals present in
According to the Brazilian Ministry of Mining and Energy wastewaters. Although the use of cow bone carbon to remove metal
(Ministério de Minas e Energia, 2009), lead produced in Brazil is a ions from wastewater is still in the research phase, the potential
byproduct of zinc mining, this country lacking economically industrial use of bone carbon systems in wastewater treatment
exploitable deposits of lead at the present time. Lead production in offers good perspectives, considering the advancements made
Brazil represents 10% of the total metallic lead consumed, supplied through research on the regeneration stage and the disposal of the
largely by recycled lead. Thus, Brazil is an importer of the semi- solid waste produced.
manufactured metal. The aim of this study was to evaluate the efficiency of the
There are various techniques available for the removal of heavy adsorption of lead onto activated carbon obtained from cow bone in
metals from aqueous effluents aimed at minimizing their impact. aqueous solutions, as an alternative to conventional processes for
Chemical precipitation is the most commonly used method in large removing heavy metals aimed at adhering to Brazilian environ-
scale and requires subsequent stages of sedimentation and filtra- mental legislation. This paper presents the kinetics and equilibrium
tion before the treated water can be reused. However, for the data, and an evaluation of the ability of isothermal and kinetic
decontamination of large volumes of effluents containing metal models to describe the process behavior. Finally, data on the
ions at low concentrations the process is unsuitable because of the desorption of the adsorbed lead from the adsorbent to enable its
low efficiency and high operating costs associated with this reuse for further adsorption are reported, aimed at obtaining a
extraction process (Nerbitt and Davis, 1994). process with a lower production of residues and greater recovery of
Other methods widely used for removing heavy metals from this heavy metal.
wastewater include ion exchange, reverse osmosis, evaporation
and membrane filtration. Many of these methods have drawbacks
2. Methods
such as high costs associated with the installation, operation and
sludge disposal, and some of them are not appropriate for small-
All reagents used were of analytical grade and the solutions
scale industries (Kobya et al., 2005). Furthermore, the identifica-
were prepared with deionized water. The lead solutions were
tion of cost-effective methods for the removal of heavy metals at
prepared with 99% lead nitrate e Pb(NO3)2 (Vetec).
low concentrations represents a difficult challenge (Cordero et al.,
2004). In this regard, the adsorption process is highly effective
and economical (Fu and Wang, 2011). For this reason, the study of 2.1. Adsorbent preparation
adsorption has grown significantly in recent years, leading to
research on the development and optimization of increasingly se- The activated carbon originating from cow bone was provided
lective adsorbents. by the company BONECHAR Activated Carbon in Brazil (Maringá-
The performance of a particular adsorbent is a function of Paraná-Brazil), and is referred to as AC in this paper. The raw ma-
several factors including the pH, temperature, metal solution con- terial is exclusively bovine and underwent a physical activation
centration and surface area of the adsorbent. It is also important to process, performed at elevated temperatures (above 800 C), under
assess the desorption capacity of the material, since through this controlled conditions, providing a high surface area, formed of
process it is possible to recover the metal, which is in a concen- uniformly distributed pores classified as micro-, medium and
trated form, and restore the adsorbent for reuse, resulting in macropores.
reduced costs and waste generation. According to data provided by the company, the AC sample has
Activated carbon is currently considered as a universal adsor- large percentages of carbonate and phosphate groups. The basic
bent for removing pollutants from contaminated water due to its character of these groups decreases the potential for the adsorption
high surface area, high adsorption capacity, fast kinetics and rela- of metal ions, since acidic pH conditions in adsorption reactions
tively easy regeneration (Sathishkumar et al., 2012). Activated enhances the release of these groups, which then interact with the
carbon is a carbonaceous material with high porosity which can be metal cation. For the removal of these interferences, the acid
applied in the treatment of various wastewaters for a variety of treatment of the carbon was performed. It is essential to under-
contaminants. It is necessary, however, to research and develop stand the factors influencing the adsorption prior to modification of
activated carbons of low cost and with alternative materials for use the adsorbent in order to adapt its specific physical and chemical
in the control of water pollution (Wang et al., 2010). The ease of properties, such as surface area, pore size and the presence of
obtaining activating carbon is also a positive factor, since any ma- different surface functional groups, and increase its affinity for the
terial with a high concentration of fixed carbon can be activated, for metals present in the water (Rivera-Utrilla et al., 2011).
instance pine knots, eucalyptus, coconut bark, palm bark, fruit pips, The preparation of the AC began with the separation of the
waste oil and animal bone. desired particle sizes (30 mesh), followed by washing in distilled
Several studies have been reported on lead adsorption with water and oven drying. The AC was subjected to acid washing in
activated carbon produced from alternative materials such as 0.2 M HNO3 at a concentration of 15 g L1 in two cycles of 3 h, then
cashew nuts (SenthilKumar et al., 2012), apricot seeds (Kobya et al., washed with distilled water at pH 3.0 0.2 (QUIMIS 400M2 pH
2005), coconut shell (Sekar et al., 2004; Song et al., 2010), hazelnut meter) and oven dried The surface of the adsorbent was modified
bark (Imamoglu and Tekir, 2008), tamarind seeds (Acharya et al., with nitric acid since the oxidizing properties can be controlled by
2009), grape seeds (Al Bahri et al., 2012), tobacco waste (Kilic the temperature and acid concentration. Furthermore, there is an
et al., 2011) and rice husks (Yalçin and Sevinç, 2000; Liu et al., increase in the removal of Pb2þ by activated carbon oxidized with
2012). Research on activated carbon of animal origin is, generally, HNO3, which may be related to the cation exchange capacity being
less common than studies on materials of plant origin, since their increased by the presence of oxygenated groups (Xu and Liu, 2008).
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8 3
2.2. Determination of surface functional groups equation of pseudo-first-order (Eq. (1)) and the linear kinetic model
of pseudo-second-order (Eq. (2)).
The methodology for determining the nature and amount of
surface functional groups of the AC was adapted from the Boehm k1 $t
logðqe qt Þ ¼ logðq1 Þ (1)
titration method (Boehm, 1994). For the determination of func- 2:303
tional groups, 0.2 g of AC were placed in contact with 50 mL of 0.1 M
HCl, NaOH, Na2CO3 and NaHCO3 in an orbital shaker (MARCONI t 1 t
¼ þ (2)
MA-410) for 24 h at 25 C with stirring at 120 rpm. Aliquots (10 mL) qt k2 $ðq2 Þ2 q2
were titrated with 0.1 M NaOH or HCl in triplicate. The number of
acid groups present on the surface of the solid was determined by
assuming that NaOH neutralizes carboxyl groups, lactones and 2.7. Adsorption isotherms
phenolics, Na2CO3 neutralizes carboxylic groups and lactones and
NaHCO3 only neutralizes carboxylic groups. The number of basic A mass of 0.10 g of AC was placed in contact with 50 mL of lead
sites was calculated considering the quantity of HCl that reacted solution in concentrations ranging from 25 to 400 mg L1, in a
with the adsorbent. water bath (MARCONI MA-410) at 25 C with stirring at 120 rpm.
The pH was adjusted to 4.0 0.3 (QUIMIS 400M2 pH meter) during
2.3. Determination of pH at the point of zero charge (pHPZC) the adsorption period, as determined in the previous test. The
samples were then filtered and the liquid phase was analyzed by
The methodology for determining the point of zero charge FAAS (SHIMADZU AA-6300). The amount of lead adsorbed at
(pHPZC) was adapted from that described by Regalbuto (Regalbuto equilibrium was calculated (in mg g1) and the adsorption pa-
and Robles, 2004) known as the “eleven point PZC measure- rameters were obtained through the linearization of the Langmuir
ment”. A mass of 0.025 g of adsorbent was placed in contact with (Eq. (3)) and Freundlich (Eq. (4)) models. The Langmuir equilibrium
25 mL of aqueous solution under 11 different conditions of initial parameter, RL, expresses the essential characteristics of the
pH (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12), adjusted with solutions of 0.1 M isotherm (Eq. (5)). For RL > 1, the isotherm is of the unfavorable
NaOH or HNO3, in a bath with stirring (MARCONI MA-410) at type; RL ¼ 1 indicates a linear isotherm; for 0 < RL < 1 the
120 rpm for 24 h at 25 C. After this step, the pH of each solution isotherm is favorable; and for RL ¼ 0 the isotherm is irreversible.
was measured (QUIMIS 400M2 pH meter) and a plot of the initial
Ce 1 Ce
pH versus the final pH was obtained. The range where the pH of the ¼ þ (3)
solution remains constant is taken as the pH at the point of zero qe kL $qm qm
charge (pHPZC).
1
lnqe ¼ lnkF þ $lnCe (4)
2.4. Metal precipitation test n
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
4 M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8
the completion of the tests, the samples were filtered and the liquid
phase was analyzed by FAAS (SHIMADZU AA-6300).
Table 1
Concentration of surface functional groups (mEq g1).
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8 5
Table 2
Kinetics constants of pseudo-first order and pseudo-second order for adsorption
obtained with the different metal concentrations studied.
K1 q1 R2 K2 q2 R2
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
6 M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8
Table 3 Table 4
Values obtained for adsorption parameters of the Langmuir and Freundlich models. Comparison between adsorption capacities of several sorbents for lead (Note: A.C.:
activated carbon).
Langmuir Freundlich
Sorbent Adsorption pH C0 Reference
qm (mg g1) 47.619 kF (L g1) 8.793
capacity (mg L1)
kL (L mg1) 0.059 1/n 0.305
(mg g1)
RL 0.263 R2 0.960
R2 0.993 Cashew nut 28.90 6.0e6.5 40 Tangjuank
shells A.C. et al., 2009.
Hazelnut husk A.C. 13.05 5.7 40 Imamoglu and
Tekir, 2008.
With respect to the Langmuir equilibrium parameter (RLÞ the Coconut shell A.C. 26.50 4.5 50 Sekar et al., 2004.
value obtained was 0.263, i.e., between 0 and 1, indicating that the Apricot stone A.C. 22.85 4.0 45 Kobya et al., 2005.
isotherm is favorable. The same favorable behavior for the 1/n ratio Van apple pulp A.C. 15.96 5.0 40 Depci et al., 2012.
Polygonum 98.39 5.0 50e75 Wang et al., 2010.
of the Freundlich isotherm was not observed. orientale A.C.
Table 4 shows a comparison between the adsorption capacities Pine cone A.C. 27.53 5.0 50e200 Mom cilovi
c
of several sorbents for lead, taken from the literature. From these et al., 2011.
results, it is possible to verify that the activated carbon obtained Cow bone A.C. 32.10 4.0 100 This study.
from cow bone has a good adsorption capacity in comparison to
other sorbents.
It can be observed that the contaminant concentration in the
3.7. Assays for lead desorption using various desorbent solutions solution increases rapidly in the first half hour, with a recovery of
approximately 60%. The concentration of the remaining lead after
Fig. 6 shows the percentages of lead removal for the six different 8 h of desorption was 45.8 mg L1.
chemical agents used in this study. Table 5 shows a comparison of the percentages of lead desorbed
HCl showed the highest efficiency, with approximately 65.5% from several different types of activated carbon using a variety of
removal in 6 h, followed in decreasing order by HNO3 (57%), H3PO4 desorbent solutions, based on data available in the literature. From
(49.9%), NaOH (14.4%), NaCl (5.8%) and distilled water (3.2%). None these results, it can be observed that the methodology used is
of the solutions used caused apparent physical changes or damage satisfactory; however, the values obtained are below those re-
to the adsorbent, enabling its reuse. ported in the literature. It should be noted that the removal effi-
Based on these findings, HCl was selected as the desorption ciency could be optimized through more detailed studies on this
agent because, besides allowing greater removal and being of low process step.
cost compared to other chemicals, the acidic medium contains After 3 h there is no change in the concentration of lead
protons which, in solution, replace the metal ions adsorbed on the recovered leading to unnecessary energy expenditure in an
carbon. The opposite effect was observed in the test performed with extended assay. Thus, 3 h was adopted as the equilibrium time for
NaOH, where there was a low recovery of Pb(II). Furthermore, the the subsequent tests.
hydrochloric acid covers the surface of the activated carbon with Hþ
ions, leaving it completely protonated for the next adsorption cycle. 3.9. Assays of adsorbent reuse
Fig. 6. Lead desorption from activated carbon using several desorbent chemical agents
Fig. 5. Langmuir and Freundlich models for the lead adsorption isotherm. (T ¼ 25 C, 120 rpm and m ¼ 0.1 g).
Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
Cleaner Production (2013), http://dx.doi.org/10.1016/j.jclepro.2013.08.020
M.A.P. Cechinel et al. / Journal of Cleaner Production xxx (2013) 1e8 7
Table 5
Comparison of lead desorption percentages of several sorbents using HCl (Note: A.C.:
activated carbon).
Acknowledgments
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Please cite this article in press as: Cechinel, M.A.P., et al., Study of lead (II) adsorption onto activated carbon originating from cow bone, Journal of
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