Int. J. Environ. Sci. Tech.

, 7 (4), 751-758, Autumn 2010

ISSN: 1735-1472 Y. B. Onundi et al.
© IRSEN, CEERS, IAU

Adsorption of copper, nickel and lead ions from synthetic

semiconductor industrial wastewater by palm shell activated carbon
Y. B. Onundi; *A. A. Mamun; M. F. Al Khatib; Y. M. Ahmed
Bioenvironmental Engineering Research Unit (BERU), Department of Biotechnology Engineering, Faculty of
Engineering, International Islamic University Malaysia, Gombak, 50728 Kuala Lumpur, Malaysia

Received 10 May 2010; revised 26 June 2010; accepted 19 July 2010

ABSTRACT: Granular activated carbon produced from palm kernel shell was used as adsorbent to remove copper,
nickel and lead ions from a synthesized industrial wastewater.Laboratory experimental investigation was carried out to
identify the effect of pH and contact time on adsorption of lead, copper and nickel from the mixed metals solution.
Equilibrium adsorption experiments at ambient room temperature were carried out and fitted to Langmuir and Freundlich
models. Results showed that pH 5 was the most suitable, while the maximum adsorbent capacity was at a dosage of 1
g/L, recording a sorption capacity of 1.337 mg/g for lead, 1.581 mg/g for copper and 0.130 mg/g for nickel. The
percentage metal removal approached equilibrium within 30 min for lead, 75 min for copper and nickel, with lead
recording 100 %, copper 97 % and nickel 55 % removal, having a trend of Pb2+ > Cu2+ > Ni2+ . Langmuir model had higher
R2 values of 0.977, 0.817 and 0.978 for copper, nickel and lead respectively, which fitted the equilibrium adsorption
process more than Freundlich model for the three metals.

Keywords: Granular activated carbon; Heavy metals; Isotherm; Sorption; Wastewater

INTRODUCTION
High concentration of heavy metals in the and membrane filtration (Georg Steinhauser, 2008).
environment can be detrimental to a variety of living Furthermore, among aforementioned treatment
species. Excessive ingestion of these metals by humans technologies, adsorption had been reported as an
can cause accumulative poisoning, cancer, nervous efficient and economic option (Skinner and Bassin,
system damage and ultimately death (Corpacioglu and 1988; Mahvi, 2008; Malakootian et al., 2009). A number
Huang, 1987; Issabayeva et al., 2007). In Malaysia, of adsorbent materials have been studied for their ability
industries dealing in electroplating, electronics, to remove heavy metals and they have been sourced
batteries and metal treatment/fabrication are the major from natural materials and biological wastes of industrial
sources of heavy metals contamination. Many of these processes (Igbinosa and Okoh, 2009). These materials
industries are located in the western coast of the including: activated carbon (Uzun and Guzel, 2000; Goel
peninsular Malaysia, which includes Klang Valley, et al., 2005; Issabayeva et al., 2007; Mondal et al., 2008),
Malacca, Johor Bahru and Penang areas (DOE, 1979). chitosan and carrageenan (Bong et al., 2004), lignite
Increased concern by environmentalists and (Allen et al., 1997), kaolinite and ballclay (Chantawong
governments on the effects of heavy metals and an et al., 2003), diatomite (Ulmanu et al., 2003), coconut
attempt to protect public health has resulted in fiber (Igwe et al. 2007) and limestone (Aziz et al., 2004).
increased research in the development of advance However, adsorption by activated carbon had been
technologies to remove heavy metals from waters and reported as a technically and economically viable
wastewaters (Bong et al., 2004; Karbassi et al., 2007; technology for heavy metal removal (Huang and
Shetty and Rajkumar, 2009; Resmi et al., 2010). Such Morehart, 1991; Bong et al., 2004).
treatment efforts involved application of unit In Malaysia, the palm oil industry generates huge
operations or unit processes such as chemical amounts of palm shell; a large portion of it is either
precipitation, coagulation, adsorption, ion exchange burned in open air or dumped in area adjacent to the
mill, which creates environmental and disposal
*Corresponding Author Email: [email protected]
Tel./Fax: +601 2365 0516
problems. Therefore, application of palm shell activated
 Y. B. Onundi et al.

carbon as an adsorbent offers highly effective Table 1: Properties of GAC adsorbents

technological means in dealing with pollution of heavy Parameters GAC
metals and solving palm shell disposal problems, with Raw material Palm Kernel Shell
Particle size (mm) 1.68 -2.38
minimum investment required (Najua et al., 2008). Ash content 4% max
Pervious works on metals removal had focused on Density (g/cm3) 0.864
single metal ions removal and little information is Surface area (m2 /g) (BET) 513.3
available on multimetal adsorption (Abdel-Ghani and Average pore size (Å) 48.5
Total pore volume (cc/g) 0.622
Elchaghaby, 2007; Abdel-Ghani et al., 2009) even Elemental analysis (%)
though most industries produce wastewater containing C 64.45
more than one metal ion in their effluent. In this work, N 23.09
O 0.00
investigation on the effect of pH, contact time and Others 32.09
dosage on metal adsorption from   a matrix of 3 metals
was carried out using palm shell based activated
carbon. While isotherm studies were used to model the GAC. The same machine was also used for the
the adsorption process. energy dispersive x-ray (EDX) spectra analysis to know
the elemental composition of the GAC. Adsorbent
MATERIALS AND METHODS samples for Fourier transform infrared (FTIR) analysis
Industrial wastewater samples from a semiconductor were prepared by diluting the GAC to 5 % in KBr and
company (located at Kuala Langat, Malaysia) were cast in disks for analysis to obtain the spectrum from a
collected for a week (8-12, June 2009), preserved and PerkinElmer precisely of model 100, earlier followed by
tested for metals content following standard method Zvinowanda et al., (2009). Specific surface area of the
(Standard Methods, 2000) procedures. The GAC was measured by an American Coulter sorptometer
concentration of heavy metals, namely lead, nickel and machine of model SA-3100, using N2 as adsorbent at the
copper in the industrial wastewater served as the bases
for the adsorption study in the laboratory. liquid nitrogen temperature of -196 °C.

Adsorbate Adsorption study

Metals solutions (copper, lead and nickel) of 1000 For each experiment, 50 mLof synthetic water sample
mg/L in nitric acid were purchased from Fisher Scientific, containing mixed metals of 2.0 mg/L Cu, 1.5 mg/L Pb
UK. Aqueous solutions of metals were prepared in the and 0.8 mg/L Ni, was prepared based on industrial
laboratory based on metal concentration in the wastewater metal concentration and added to a
industrial effluent. Each metal solution was diluted with calculated amount of adsorbent in 100 mL shake flask.
distilled water to obtain the desired initial The pH adjustment of solution was done using 1.0 M
concentration, to mimic the industrial wastewater. HCL and 1.0 M NaOH. The adsorbent in solution was
agitated in a mechanical shaker at a speed of 100 rpm at
Adsorbent 27 °C (± 2). Blank solutions were treated similarly
The palm shell based granular activated carbon without the adsorbent and under control condition.
(GAC) was listed in Table 1 used as an adsorbent for The solution was filtered using a Whatman® 0.45µm
this research was bought from KD Technology filter paper. The results were analyzed for the residual
Malaysia. The adsorbent was washed with distilled concentration of metals in the filtrate by atomic
water to remove fines and dirt following the procedure adsorption spectrophotometer (PerkinElmer HGA900).
of Goel et al. (2005). The wet material was then dried at Equilibrium concentration of metals at different
110 °C for 6 h before characterization was done and adsorbent dosage (1, 2, 3, 4 g/L), at ambient temperature
used in the adsorption studies at ambient room was used for the isotherm study. The adsorption
temperature of 27 °C (± 2). capacity of adsorbent was calculated using Eq.1.
(C 0 − C t ).V (1)
Adsorbent characterization qt =
m
Scanning electron microscope (SEM) (JSM-5600
model) machine of the Japanese manufacturer (JEOL Where, q t is the adsorption capacity of the
Ltd.) was employed to check the surface morphology of adsorbent at time t (mg adsorbate/g adsorbent); Co is

752
 Int. J. Environ. Sci.
Y. Tech.,
B. Onundi
7 (4),et751-758,
al. Autumn 2010

the initial concentration of metal (mg/L); Ct is the Effect of pH on adsorption

residual concentration of metal after adsorption had The uptake and percentage removal of metals from
taken place over a period of time t (mg/L); V is volume the aqueous solution are strongly affected by the pH
of metal solution in shake flask (L) and m is mass of of the solution (Horsfall and Abia, 2003; Zvinowanda
adsorbent (g) (Metcalf and Eddy, 2003). The metal et al. 2009). Fig. 3 shows the effect of pH variation on
removal percentage (R %) was calculated using Eq. 2. adsorption of copper, nickel and lead ions on GAC
(C 0 − C t ).100
surface. The uptake of Cu, Ni and Pb increased from
R (%) = (2) 0.095 mg/g to 0.685 mg/g; 0.045 mg/g to 0.137 mg/g and
C0

Where (R %) is the ratio of difference in metal

concentration before and after adsorption.

RESULTS AND DISCUSSION

Physical and chemical characterization of adsorbent
The SEM image of Fig. 1 reveals the porous structure
of the GAC surfac. The FTIR spectra of GAC are shown
in Fig. 2, while a summary of the peaks and their assignment
are in Table 2. As can be inferred from the FTIR analysis,
the acidic functional groups present on GAC surface were:
carboxyl, carbonyl, lactones and sulphur groups. These
groups had been reported to enhance metals adsorption
(Zhang et al., 2009; Edwin, 2008; Goel et al., 2005).
Specifically sulphur groups were reported by Goel et al,
(2005) as aiding lead ions adsorption. Fig. 1: SEM image of GAC surface

0.1501
0.145
0.140
0.135
0.130
0.125
3730.98
0.120
0.115 2335.94
3853.79
Absorbance (g/L)

2008.39
0.110 2151.42 571.86
0.105 3645.97 2224.61 702
3563.93 490.61
0.100
0.095 1557
0.090 1104 439.23
0.085
0.080
0.075
0.070
0.065
0.060
0.0553
4022 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400

cm-1

Fig. 2: FTIR spectrum of GAC

753
 Y. B. Onundi
Adsorption of heavy et al.
metals by activated carbon

0.111 mg/g to 0.493 mg/g, respectively when the Furthermore, the low solubility of hydrolyzed metal
solution’s pH was increased from 2 to 5. For pH values species may be another reason for maximum adsorption
above 5, the adsorption capacity decreased with in this pH range.
increment in pH. The mechanism of metals adsorption
by the adsorbent with pH variation could be explained Effect of contact time
with the same concept as put forward by Corapcioglu The relationship of percentage metals removal by
and Huang (1987), Bansal and Goyal (2005), Najua et adsorbent with contact time was plotted and presented
al. (2008) and that in the pH range of 2 to 3, copper, in Fig. 4. The amount of the adsorbed metal ions
lead and nickel ions would be present predominately increased as the time lapses, similar case was recorded
as M(II) ions. The minimum adsorption observed at by Gueu, et al., (2007). The adsorbent showed a rapid
low pH of 2 could be, on one hand due to the fact that metal reduction for the first 5 min of contact time, with
the presence of higher concentration and higher further increase in time the sorption kinetics decreased
mobility of H+ ions favoured H+ adsorption compared progressively. The percentage metal removal
to M (II) ions and on the other hand due to the high approached equilibrium within 30 min for Pb and 75
solubility and ionization of metals salt in the acidic min for Cu and Ni. The fast adsorption at the initial
medium. It would be plausible to suggest that at lower stage was probably due to the initial concentration
pH value, the surface of the adsorbent is surrounded gradient between the adsorbate in solution and the
by hydronium ions (H+), thereby preventing metals ions number of vacant sites available on the GAC surface at
from approaching the binding sites of the adsorbents. the beginning. The progressive increase in adsorption
At higher H+ concentration, the adsorbents surface and consequently the attainment of equilibrium
becomes more positively charged such that the adsorption may be due to limited mass transfer of the
attraction between adsorbents and metal cations is adsorbate molecules from the bulk liquid to the external
reduced. In contrast, as the pH increases, more surface of GAC. It was noted that the sorption capacities
negatively charged surface becomes available thus
facilitating greater metals removal. It could be deduced Table 2: Peaks from GAC spectrum and their possible assignment
that the sorption of metal cations increased with GAC Band
Possible assignments
increasing pH as the metal ionic species become less position/cm
3564 O-H stretching (intermolecular diametric)
stable in the solution. The maximum adsorption 3200-2800 C-H stretching (alkenes)
observed in the pH range of 4.5 to 6 might be due to 2151 C=N stretching (alkynes)
partial hydrolysis of metal ions, resulting in the 1697 C=O Stretching (aldehydic)
formation of M (OH)+ ions and M(OH)2, which would 1104 S-O Stretching (sulfates)
be adsorbed to a greater extent on a less-polar carbon 1125 C-H Amines
680-610 S-O Bends (sulfates)
surface of the adsorbents compared to M2+ ions.
 
0.80
Adsorption Capacity for Cu (mg/g)

0.70

0.60

0.50

0.40

0.30

0.20

0.10

0.00
0 2 4 6 8 10 12
P H Va lue

Cu Ni Pb

Fig. 3: Effect of pH on adsorption of metals onto GAC from a mixed metals solution

754
 Int. J. Environ. Sci. Y.Tech., 7 (4), 751-758,
B. Onundi et al. Autumn 2010

corresponding to equilibrium varied for each metal, with Effect of adsorbent dosage
lead recording 100 %, copper 97 % and nickel 55 %, The effect of variation of GAC dosage on amount of
giving a trend of Pb > Cu > Ni on the adsorbent. It was metal adsorbed is shown in Fig. 5. A trend of increment
assumed that the acidic groups on the GAC had affinity in adsorption capacity with increment in adsorbent
for the three metals; the observed trend was probably dosage was observed from 0.5 g/L to 1 g/L. Adsorbent
due to the sulphate group on the adsorbent having recorded a maximum capacity of 1.581 mg/g for copper,
higher affinity for lead ions, making lead reach equilibrium 1.337 mg/g for lead and 0.130 mg/g for nickel at 1 g/L
concentrations faster than copper and nickel ions. The dosage. Further increment of adsorbent above 1 g/L
higher initial concentration of copper also favored resulted in a decline in adsorption capacity.The initial
copper over nickel in the percent uptake achieved by 75 increment in adsorption capacity with increase in
min. It is plausible to assume that the lower concentration adsorbent dosage was expected, since number of
of nickel probably did not favor nickel competition with adsorbent particles increases and thus more surface
lead and copper for the same available adsorption site on areas were available for metals attachment. Same trend
the GAC surface, which resulted in the comparable lower was reported by Dakiky et al. (2002), Acharya et al.,
amount of nickel removal before equilibrium was attained. (2009).

120.0

100.0

80.0
Removal (%)

60.0

40.0

20.0

0.0
0 20 40 60 80 100 120 140
Tim e (m in)
Cu Ni Pb

Fig. 4: Effect of conta ct time on a dsorption of Cu (II), Ni (II) and Pb (II)

(at ambient temperature =27 (±2)°C, adsorbent dose = 4 g/L, pH = 5).

1.80
Adsorption Capacity for Ni (mg/g)

1.60
1.40

1.20

1.00
0.80

0.60
0.40
0.20

0.00
0 1 2 3 4 5
Ads oAdsorbent
rbe nt Do sdosage
a ga (g/L)
(g/L)

Ni GAC (P b) Cu

Fig. 5: Effect of adsorbent dosage (g) variation on metals adsorption (at pH5,
agitation period of 75 min at 100 rpm)

755
 Y. B. Onundi et al.

It is plausible to suggest that with higher dosage of solution at equilibrium (g/L); x is the mass of
adsorbent there would be greater availability of contaminant adsorbed (g); m is the mass of solid
exchangeable sites for metal ions as noted by Babel sorbent (g) a and n are empirical coefficients; a
and Kurniawan (2004) and Najua et al. (2008). Further (mg/g) in the Langmuir equation is indicative of the
increment in adsorbent dosage beyond maximum relative adsorption capacity of the adsorbent. The
adsorption capacity at 1 g/L resulted in a decline in constant b is the saturation coefficient (m3/g) and
capacity as shown in Fig. 5. This reduction in capacity Kf is the Freundlich constant indicative of the
had been explained as due to the overlapping of the relative adsorption capacity of the adsorbent (mg/
adsorption sites as a result of overcrowding of g).The constant 1/n indicates the tendency of the
adsorbent particles beyond 1 g/L dose (Garg et al., adsorbate to be adsorbed (Bishop, 2004; Goel et al.,
2003; Najua et al., 2008). Moreover, the high adsorbent 2005). The estimated model parameters with
dosage could impose a screening effect on the dense correlation coefficient (R2) for the two models are
outer layer of the cells, thereby shielding the binding shown in Table 3. It was observed that results fitted
sites from metals (Pons and Fuste, 1993). better in the Langmuir model in terms of R2 value,
recording 0.978 for lead, 0.977 for copper and 0.817
Equilibrium adsorption isotherms
for nickel. The affinity of the metals for the adsorbent
Several models had been used in literatures to
surface in terms of value “b” in the Table 3 varied in
describe the experimental data of adsorption isotherms.
the trend Pb > Cu > Ni, which is in agreement with the
The Freundlich (Freundlich and Hatfield, 1926) and
Langmuir (Langmuir, 1918) models are the most frequently trend in Fig. 4. It was assumed that this trend was
employed models, these two models were used in the due to the presence of sulphate acidic group present
present work. Equilibrium data obtained were fitted to on the GAC surface. It was observed that the trend of
the Langmuir and Freundlich isotherms. The following adsorption capacity in terms of constant “a” was Cu
expressions of straight line were found by means of > Pb > Ni. This was probably due to the initial
mathematical transformation of isotherms equation. concentration of metals following same trend and this
Langmuir isotherm is shown as Eq.3: trend is inline with trend in Figs. 3 and 4. It could be
inferred from this result that the trend of constant
1 1 + bc e 1 1 “b” was due to sulphate group present on the GAC,
cs = = = + (3)
x abc e a abc e it also made Pb have higher affinity for the GAC
m
surface, making it reach equilibrium concentration
Freundlich isotherm is shown as Eq. 4:
x 1 within 30 min of contact time, while Cu and Ni took
log( ) = log K f + log C e longer time as was observed in Fig. 4. However, the
m n (4)
higher initial concentration of copper favored copper
Where, Cs is the amount of contaminant sorbed in total metal adsorbed on the GAC as shown in the
on the solid per unit of solid (mg sorbate/g sorbent), trend of Fig. 5, which also explains the trend of
Ce is the concentration of contaminant remaining in constant “a” in Table 3.

Table 3: Isotherm parameters for metals adsorption at 27 (±2) °C and pH 5

Metals Equation Constants Cs (Equation) R²
x (1.263)(57 .519 )
Langmuir a =1.263 b=57.519 cs = = 0.977
m 1 + 57.519C e
Copper
x
Freundlich Kf =0.228 n=3.777 c s = = 0.228.ce1 / 3.777 0.581
m
x (0.261)( 2.2951)
Langmuir a = 0.261 b=2.2951 cs = = 0.817
m 1 − 2.2951Ce
Nickel
x
Freundlich Kf =-0.607 n=1.29927 cs = = −0.607.ce1/ 1.29927 0.761
m
x ( 0841)(80389.61)
Langmuir a = 0.841 b=80389.61 cs = = 0.978
m 1 + 80389.61C e
Lead
x
Freundlich Kf = 0.112 n=8.4295 cs = = 0.112.ce1/ 8.4295 0.709
m

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 Y. B.Tech.,
Int. J. Environ. Sci. Onundi et 751-758,
7 (4), al. Autumn 2010

CONCLUSION Bansal, R. C.; Goyal, M., (2005). Activated carbon adsorption.

It was observed that copper, nickel and lead ions London, Taylor and Francis Group, 351-353.
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at pH 5, while the maximum adsorbent dosage was Bong, K. P.; Seung, H. S.; Young, J. Y., (2004). Selective
1 g/L recording a sorption capacity of 1.337 mg/g for biosorption of mixed heavy metal ions using polysaccharides.
lead, 1.581 mg/g for copper and 0.130 for nickel. The Korean J. Chem. Eng., 21 (6), 1168-1172 (5 pages) .
Chantawong,V.; Ha rvey, N. W.; Bashkin, V. N., (2 003 ).
metal removal approached equilibrium within 30 min Comparison of heavy metals adsorption by T hai Ka olin
for Pb, 75 min for Cu and Ni of contact time. Langmuir and Ballclay. Water, Air, Soil Pollut., 148 (1-4), 111-125
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for copper, nickel and lead respectively fitted the Corapcioglu, M. O.; Huang, C. P., (1987). The adsorption of
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model for the three metals. From the isotherm Dakiky, M.; Khamis, M.; Manassra, A.; Mer’eb, M., (2002).
constants, it was observed that the trend of metals Selective a dsorption of chromiu m (VI) in industrial
affinity for GAC surface was Pb > Cu > Ni, while the wastewater using low-cost abundantly available adsorbents.
Adv. Environ. Res., 6 (4), 533-540 (8 pages) .
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The authors wish to acknowledge the Endowment Chemistry. Methuen and Co. Ltd., London.
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Fund Type A of International Islamic University (IIUM) removal from aqueous solution by adsorption on treated
for funding the research. Assistance from all members sawdust. Bioresour. Tech., 89 (2), 121-124 (4 pages) .
of Nanoscience and Nanotechnology Research Group Georg Steinhauser, M. B., (2008). Adsorption of ions onto
(NANORG) and Bio-environmental Research Unit high silica volca nic glass. Appl. Ra d. Iso., 66 (1), 1 -8
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(BERU) of the Faculty of Engineering IIUM is very Goel, J.; Krishna, K.; Chira, R.; Vinod, K., (2005). Removal of
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AUTHOR (S) BIOSKETCHES

Onundi, Y. B., M.Sc., Department of Biotechnology Engineering, International Islamic University Malaysia, P.O.Box 10, 50728 Kuala
Lumpur, Malaysia., Kuala Lumpur, Malaysia. Email: [email protected]

Mamun, A. A., Ph.D., Department of Biotechnology, Faculty of Engineering, International Islamic University Malaysia (IIUM), Jalan
Gombak, 53100 Kuala Lumpur, Malaysia, Kuala Lumpur, Malaysia. Email: [email protected]

Al Khatib, M. F., Ph.D., Department of Biotechnology, Faculty of Engineering, International Islamic University Malaysia (IIUM), Jalan
Gombak, 53100 Kuala Lumpur, Malaysia, Kuala Lumpur, Malaysia. Email: [email protected]

Ahmed, Y. M., M.Sc., Department of Biotechnology, Faculty of Engineering, International Islamic University Malaysia (IIUM), Jalan
Gombak, 53100 Kuala Lumpur, Malaysia, Kuala Lumpur, Malaysia. Email: [email protected]

How to cite this article: (Harvard style)

Onundi, Y. B.; Mamun, A. A.; Al Khatib, M. F.; Ahmed, Y. M., (2010). Adsorption of copper, nickel and lead ions from synthetic semiconductor
industrial wastewater by palm shell activated carbon. Int. J. Environ. Sci. Tech., 7 (4), 751-758.

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