DOI: 10.1002/tqem.21536
R E S E A R C H A R T I C L E
Experimental investigation of adsorption capacity of anthill
in the removal of heavy metals from aqueous solution
Adeyinka Sikiru Yusuff Idowu Iyabo Olateju
Department of Chemical and Petroleum Engi-
neering, College of Engineering, Afe Babalola
University, Ado-Ekiti, Nigeria
Correspondence
Adeyinka Sikiru Yusuff, Department of Chemical
and Petroleum Engineering, College of Engineer-
ing, Afe Babalola University, Ado-Ekiti P.M.B.
5454, Nigeria.
Email: [email protected]
Abstract
In the present work, the adsorption capacity of anthill was investigated as a low-cost adsorbent
to remove the heavy metal ions, lead (II) ion (Pb2+), and zinc (II) ion (Zn2+) from an aqueous solu-
tion. The equilibrium adsorption isotherms of the heavy metal ions were investigated under batch
process. For the study we examined the effect of the solution’s pH and the initial cations con-
centrations on the adsorption process under a fixed contact time and temperature. The anthill
sample was characterized using a scanning electron microscope (SEM), X-ray fluorescence (XRF),
and Fourier transform infrared (FTIR) techniques. From the SEM analysis, structural change in the
adsorbent was a result of heavy metals adsorption. Based on the XRF analysis, the main compo-
sition of the anthill sample was silica (SiO2 ), alumina (Al2 O3 ), and zirconia (ZrO2 ). The change in
the peaks of the spectra before and after adsorption indicated that there was active participation
of surface functional groups during the adsorption process. The experimental data obtained were
analyzed using 2- and 3-parameter isotherm models. The isotherm data fitted very well to the 3-
parameter Radke–Prausnitz model. It was noted that Pb2+ and Zn2+ can be effectively removed
from aqueous solution using anthill as an adsorbent.
K E Y W O R D S
adsorption, anthill, characterization, equilibrium isotherm, heavy metal
1 I N T R O D U C T I O N
Indiscriminate disposal of wastewater containing heavy metals has
received considerable attention in recent years, primarily due to the
fact that their presence in waste stream can be readily adsorbed by
aquatic organisms and make them directly enter the human food chain,
thus posing a serious health risk to consumers (Lin, MacLean, & Zeng,
2000). Because of the ability of heavy metals to accumulate in living
tissues and because they cause damage to these tissues over time,
heavy metals are classified as carcinogens. For example, exposure to
lead ions can cause anemia, kidney damage, and even untimely death
(Mohammed-Ridha, Ahmed, & Raoof, 2017), while zinc ions at elevated
concentration result in pancreas damage, osteoporosis, and even death
(Wahi, Ngaini, & Jok, 2009). Water or wastewater containing heavy
metals requires effective treatment techniques that can completely
remove these toxic metals (Yusuff, 2017).
A number of treatment techniques for the removal of heavy
metals from waste solution have been reported. These techniques
include chemical precipitation, ion exchange, membrane separation,
the Fenton-biological method, ultrafiltration, electrochemical degra-
dation, and adsorption. Among these methods, adsorption of adsor-
bate from fluid onto porous solid material called adsorbent has been
identified as a simple and economical technique (Yusuff, 2017). Adsor-
bent plays an important role in the adsorption process as it serves
as a site for the separation of adsorbate from the fluid. However, the
unique feature of an adsorbent is its adsorption capacity, which is
usually influenced by the material used and method adopted for its
production (Hameed, Krishni, & Sata, 2009). This is because the adsor-
bent source and its preparation conditions will influence its physi-
cal, chemical, and morphological properties. Many adsorbents derived
from different sources such as agricultural waste (Yusuff, Olateju, &
Ekanem, 2017), naturally occurring materials (Mohamed, Abdelka-
rim, Ziat, & Mohamed, 2016), and microorganism (Mohammed-Ridha
et al., 2017) just to mention but a few that have been used for the
removal of heavy metals from wastewater. In this present work how-
ever, anthill, a form of siliceous fireclay, was used as a low-cost adsor-
bent for the removal of heavy metals from aqueous solution due to its
ready availability in Nigeria. According to Akinwekomi, Omotoyinbo,
and Folorunso (2012), anthill sample contains metal oxides such as sil-
ica (SiO2 ), alumina (SiO2 ), iron oxide (Fe2 O3 ), and the like. However,
some of these metal oxides in their pure or composite forms have been
used as adsorbents for the removal of contaminants from wastewa-
ter (Eletta, Ajayi, Ogunleye, & Akpan, 2016; Fisli, Ridwan, Krisnandi, &
Gunlazuardi, 2017). This is the main reason why anthill was chosen as
Environ Qual Manage. 2018;27:53–59. c© 2018 Wiley Periodicals, Inc. 53wileyonlinelibrary.com/journal/tqem
54 YUSUFF A N D OLATEJU
an adsorbent for the removal of cations from aqueous solution for the
present study. Furthermore, to the best of our knowledge, no literature
on the adsorption behavior of anthill for the removal of heavy metals
from aqueous solution is reported. Thus, in this present study, an anthill
sample was thermally activated, characterized, and employed as adsor-
bent to remove lead (Pb2+) and zinc (Zn2+) ions from aqueous solu-
tion. The effects of process parameters affecting the adsorption pro-
cess, such as medium pH and initial heavy metal concentrations, were
investigated. An equilibrium adsorption isotherms study was also car-
ried out and discussed in details.
2 M AT E R I A L S A N D M E T H O D S
2.1 Materials
The anthill sample used in this study was harvested from a type II
anthill situated behind the University’s staff quarters, Afe Babalola
University, Ado-Ekiti, Nigeria. All chemical reagents and materials used
in this study were of analytical grade. About 1,000 milligrams per liter
(mg/L) stock solutions of Pb2+ and Zn2+ were prepared separately
by dissolving 3.09 grams (g) of lead nitrate (Pb(NO3 )2 ) and 4.43 g
of zinc sulfate (Zn(SO4 )) in 1 liter (L) of distilled water each. From
this prepared stock solution, the desired initial concentrations of each
heavy metal ion was prepared for each run, and the concentration
was analyzed using atomic absorption spectrophotometer (AAS, Buck
Scientific 210VGP, USA).
2.2 Adsorbent preparation and characterization
The harvested anthill sample was ground by a mechanical grinder into
a fine powder. Thereafter, the fine anthill powder was passed through a
sieve mesh of 0.5 millimeter to obtain an even finer powder. The anthill
powder was then calcined in a muffle furnace at a temperature of 900
degrees Celsius (â—¦C) for 2 hours. The adopted heating rate was 10â—¦C
per minute, and after the calcination time was attained, the calcined
anthill sample was immediately removed from the furnace before its
temperature dropped to room temperature. The activated anthill sam-
ple was then kept in a sealed glass bottle to prevent contamination
with atmospheric moisture. The morphology and topography of the
adsorbent before and after adsorption was examined by scanning elec-
tron microscope (SEM-JEOL-JSM 7600F). Fourier transform infrared
(FTIR) analysis was carried out on both thermally treated and used
adsorbents in order to identify various surface functional groups and
compared, by using FTIR spectroscope (FTIR-IR Affinity-1S Shimadzu,
Japan). Moreover, the chemical compositions of the anthill samples
before and after adsorption were determined by X-ray fluorescence
machine.
2.3 Batch equilibrium studies
The batch adsorption process was carried out by bringing into con-
tact the thermally activated anthill adsorbent with an aqueous solution
containing a mixture of Pb2+ and Zn2+ in a set of conical flasks of 250
milliliters capacity each. The flasks were agitated in a temperature-
controlled water bath shaker (SearchTech Instrument) operating at a
constant stirring speed of 150 revolutions per minute. The adsorp-
tion process was conducted under the following operating condi-
tions: the pH of the aqueous solution was variously 3, 4, 5, 6, 7, 8,
and 9, and the initial Pb2+ and Zn2+ concentrations were 10, 20,
30, 40, 50, and 60 mg/L at a fixed temperature of 35â—¦C for 90 min-
utes equilibrium contact time. After equilibrium was attained, each
sample was filtered to obtain solution containing un-adsorbed Pb2+
and Zn2+ that was free of the adsorbent, and the concentration of
each metal ion was analyzed by atomic absorption spectrophotome-
ter (AAS, Buck Scientific 210VGP, USA). The removal percentage,
EA (%), and the amount of metal ions adsorbed at equilibrium, qe
in milligrams per gram (mg/g), of each metal ion were calculated as
follows:
EA =
(
Co − Ce
)
Co
× 100% (1)
qe =
(
Co − Ce
)
V
W
(2)
where Co and Ce (mg/L) are the initial concentration and concentration
at equilibrium, respectively. V (L) is the volume of the solution and W (g)
is the mass of activated anthill adsorbent.
3 R E S U LT S A N D D I S C U S S I O N
3.1 Adsorbent characterization
The SEM images of the prepared activated anthill before and after
adsorption of Pb2+ and Zn2+ are shown in Exhibit 1a and 1b, respec-
tively. As can be seen in Exhibit 1a, it is obvious that the thermally
treated anthill possesses different layers of pores on its surface, which
paves the way for heavy metals to be adsorbed. However, some of
the pores were blocked due to adsorption of cations on the activated
anthill as can be seen in Exhibit 1b.
The chemical composition analysis of prepared activated anthill
before and after adsorption as shown in the table in Exhibit 2 revealed
that silica (SiO2 ) constitutes the largest percentage in the anthill sam-
ple, followed by alumina (Al2 O3 ) and zirconia (ZrO2 ). However, the
percentage of SiO2 and Al2 O3 decreased after the adsorption pro-
cess, as can also be seen in Exhibit 2. This implies that SiO2 and Al2 O3
are identified adsorption sites in anthill, and their reduction in total
composition after the adsorption process could also be attributed to
the fact that the SiO2 surface contained silanoh (OH group), which
can interact with Pb2+ and Zn2+ (Fisli et al., 2017). A similar observa-
tion was reported for the adsorption of Pb2+, Cu2+, and Zn2+ on soil
(Lim & Lee, 2015). This is corroborated by the FTIR analysis. Further-
more, the good adsorption capacity exhibited by the thermally treated
anthill sample can also be attributed to the interaction among the
metal oxides in the adsorbent as they create several adsorption sites
for the adsorbates.
YUSUFF A N D OLATEJU 55
EXHIBIT 1 SEM images of prepared anthill adsorbent (a) before and (b) after adsorption of Pb2+ and Zn2+ [Color figure can be viewed at wiley-
onlinelibrary.com]
E X H I B I T 2 X-ray fluorescence results of prepared activated anthill
before and after adsorption process
Chemical composition
(wt%)
Before
adsorption
After
adsorption
SiO2 58.2 51.0
Al2 O3 21.6 18.3
Fe2 O3 2.36 2.66
MgO 4.77 4.72
Na2 O 4.13 4.24
K2 O 0.95 3.91
CaO 0.64 1.10
ZrO2 6.99 12.4
Other 1.20 3.57
The functional groups present on the surface of the prepared adsor-
bent before and after adsorption process were identified by FTIR
analysis, and their spectra are shown in the table in Exhibit 3. Upon
the adsorption process, some of the spectra in activated anthill shifted,
vanished, and new peaks were formed. The difference in the FTIR
spectrum obtained for the prepared activated anthill before and after
adsorption is an indication that there was participation of the surface
functional groups during adsorption process (Yusuff, 2017).
3.2 Effect of process parameters on heavy metals
removal
3.2.1 Effect of pH
The adsorption of Pb2+ and Zn2+ as a function of the hydrogen ion
concentration contained in aqueous solution was examined over a pH
range of 3 to 9 as shown in Exhibit 4. The removal percentage of
both cations decreased with increased pH of the aqueous solution. For
both Pb2+ and Zn2+, the maximum removal percentage was attained
at a pH of 5. The result obtained herein indicates that the adsorp-
tion by the anthill of Pb2+ and Zn2+ would be enhanced at a low
pH. Similar observations were reported for Pb2+ onto low-cost bio-
sorbent (Mohammed-Ridha et al., 2017) and for Zn2+ onto soil (Lim
& Lee, 2015). The maximum removal percentage of the heavy met-
als recorded for an acidic medium could be the result of interaction
between cations in solution and functional groups on the adsorption
sites of anthill (Chiban, Lehutu, Sinan, & Carja, 2009).
E X H I B I T 3 The major absorption band and assignment for anthill adsorbent before and after adsorption
Wavenumber (cm−1 )
Infrared band Before adsorption After adsorption Assignment/Vibration mode
1 3,747.69 – Si-OH (silanol) vibration mode
2 – 3,693.68 Si-Si-OH or Al-Al-OH stretching vibration
3 1,649.14 1,649.14 H-OH deformation vibration
4 1,085.92 1,105.21 -Si-O stretching
5 – 1,029.99 -Si-O stretching of clay vibration
6 – 914.26 Al-Al-OH deformation
7 785.03 786.96 Al-Mg-OH vibration of clay sheet or O-Si-O deformation vibration
8 688.59 692.44 Coupled Al-O and Si-O out of the plane
9 – 538.14 -Al-O-Si deformation
10 468.70 462.92 Si-O-Al deformation vibration
56 YUSUFF A N D OLATEJU
EXHIBIT 4 Effect of pH on removal percentage of Pb2+ and Zn2+
at fixed initial heavy metal concentration = 50 mg/L, adsorbent
dosage = 0.2 g, and temperature = 35â—¦C
EXHIBIT 5 Effect of initial concentration on removal percentage
of Pb2+ and Zn2+ at fixed pH = 5, adsorbent dosage = 0.2 g, and
temperature = 35â—¦C
3.2.2 Effect of initial concentration of heavy metals
The effects of the initial concentrations of Pb2+ and Zn2+ on their
removal percentages by thermally treated anthill was studied by
considering various values of initial concentrations between 10 and
60 mg/L. It was noticed that the removal percentage of cations
decreased from 95% to 84.2% and from 93% to 70% for Pb2+ and
Zn2+, respectively, by increasing the initial concentrations from 10
to 60 mg/L as shown in Exhibit 5. This observation revealed that
the adsorbent dosage of 0.2 g provided enough active bonding sites
for the adhesion of metal ions when the initial concentration was
10 mg/L. However, increasing the initial cations concentrations cause
the active bonding sites to become saturated, and the adsorbent capac-
ity becomes exhausted due to non-availability of adsorption sites
(Wang & Wang, 2007).
3.2.3 Adsorption isotherm
In a bid to quantify the amount of adsorbed heavy metals onto acti-
vated anthill at equilibrium conditions, two- and three-parameter
isotherm models were employed. However, the parameters contained
in the selected isotherm models are evaluated by non-linear curve
fitting, using Excel Solver and the isotherm model that best describes
the experimental results is chosen based on the correlation coefficient
(R2 ). The experimental data are assumed to be well-predicted by the
model the closer the R2 value comes to unity.
3.2.4 Two-parameter isotherm model
In this present work, the experimental data for Pb2+ and Zn2+ adsorp-
tion onto activated anthill were fitted to two-parameter isotherm mod-
els, the Langmuir and the Freundlich models. The Langmuir and Fre-
undlich isotherm models are given in Equations (3) and (4), respec-
tively, as follows:
qe =
qmax bCe
(1 + bCe)
(3)
qe = kF C
1∕n
e (4)
where qe (mg/g) is the amount of metal ions adsorbed at equilib-
rium; Ce (mg/L) is the equilibrium concentration of metal in solu-
tion; qmax (mg/g) is the maximum adsorption capacity; b is the
Langmuir equilibrium constant; kF (mg/g (L/mg)
1/ n ) indicates the
adsorption capacity of the adsorbent; and n is an adsorption
intensity.
A dimensionless constant referred to as separation factor (RL ) is
applied to ascertain the nature of adsorption by using the Langmuir
equilibrium constant (b) and the highest initial concentration of Pb2+
and Zn2+ (Co , mg/L), as given in Equation (5).
RL =
1
(
1 + bCO
) (5)
The separation factor (RL ) can either indicate irreversible adsorp-
tion (RL = 0), favorable adsorption (0 < RL < 1), linear adsorption
(RL = 1), or unfavorable adsorption (RL > 1).
From the non-curve fitting analysis shown in Exhibit 6a and 6b, the
parameters contained in both the Langmuir and the Freundlich mod-
els were determined and are presented in the table in Exhibit 7. Based
on the value of R2 , Freundlich isotherm provides the best fit to the
adsorption equilibrium data of Pb2+, while the adsorption of Zn2+ onto
activated anthill was best described by the Langmuir isotherm model.
A similar observation was reported for adsorption of Pb2+, Cd2+, and
Zn2+ onto NALCO plant sand (Mohapatra, Khatun, & Anand, 2009).
However, the values of separation factor (RL ) obtained for both Pb
2+
and Zn2+ were less than 1 as can be seen in Exhibit 7, thus suggesting
a favorable adsorption process. Furthermore, by comparing the maxi-
mum adsorption capacities of Pb2+ and Zn2+ on different adsorbents
as shown in the table in Exhibit 8, activated anthill is found to pos-
sess relatively high adsorption capacity, and this implies that it could
be regarded as an effective and low-cost adsorbent for the removal
of heavy metals from aqueous solution, especially when compared
with other forms of clay such as Agbani clay (0.65 mg/g) (Dawodu,
Akpomie, & Ejikeme, 2012) and bentonite clay (5.07 mg/g) (Oludotun,
2015).
3.2.5 Three-parameter isotherm model
For further analyses of the acquired experimental data, three-
parameter isotherm models, the Sip and Radke–Prausnitz, were
YUSUFF A N D OLATEJU 57
EXHIBIT 6 Two-parameter isotherm models for adsorption of (a) Pb2+ and (b) Zn2+ onto activated anthill
E X H I B I T 7 Two-parameter isotherm parameters and correlation
coefficients for adsorption of Pb2+ and Zn2+ onto activated anthill
Isotherm Pb2+ Zn2+
Langmuir
qmax (mg/g) 11.44 8.39
b (L/mg) 0.119 0.09
R2 0.9807 0.9842
RL 0.123 0.156
Freundlich
kF (mg/g (L/mg)
1/ n ) 1.53 1.04
n 1.62 1.76
R2 0.9903 0.9783
employed. The Sip and Radke–Prausnitz models are given in
Equations (6) and (7), respectively. All of the parameters contained in
these two models (evaluated by the non-linear analysis method) and
correlation coefficient (R2 ) are presented in Exhibit 9. However, the
plots of qe against Ce , which display the non-linear regression of the
three-parameter isotherm models to the experimental results, and
also provide solutions to those models, are depicted in Exhibit 10a and
10b. Based on the value of R2 , the Radke–Prausnitz isotherm model
provides a better fit to the isotherm data than the Sip model.
qe =
q
Ms
max(KS Ce)
1 + (KS Ce)
(6)
qe =
qmax KRP Ce
(
1 + KRP Ce
)MRP
(7)
where qe (mg/g) is the amount of metal ions adsorbed at equilib-
rium; Ce (mg/L) is the equilibrium concentration of metal in solution;
qmax (mg/g) is the maximum adsorption capacity; KS and KRP are the Sip
and the Radke–Prausnitz equilibrium constants, respectively; and MS
and MRP are Sip and Radke–Prausnitz model exponents, respectively.
E X H I B I T 8 Comparison of adsorption capacities of different
adsorbents for Pb2+ and Zn2+
Adsorption
capacity (mg/g)
Adsorbent Pb2+ Zn2+ Reference
Anthill 11.44 8.39 Present work
Red mud – 14.51 Gupta and Sharma,
2002
Calcareous soil – 4.587 Mesquita and e Silva,
1996
Agbani clay 0.65 – Dawodu et al., 2012
Nalco plant sand 21.78 58.28 Mohapatra et al.,
2009
Acid soil – 6.004 Arias, Pérez-Novo,
López, and Soto,
2006
Waste beer yeast 2.34 – Parvathi, Nagendran,
and Nareshkumar,
2007
Bentonite clay 5.07 – Oludotun, 2015
E X H I B I T 9 Three-parameter isotherm parameters and correlation
coefficients for adsorption of Pb2+ and Zn2+ onto activated anthill
Isotherm Pb2+ Zn2+
Sip
qmax (mg/g) 222.05 126.44
KS 0.00035 0.00027
MS 0.626 0.583
R2 0.9927 0.9769
Radke–Prausnitz
qmax (mg/g) 242.71 153.73
KRP 0.051 0.059
MRP 0.381 0.431
R2 0.9932 0.9782
58 YUSUFF A N D OLATEJU
EXHIBIT 10 Three-parameter isotherm models for adsorption of (a) Pb2+ and (b) Zn2+ onto activated anthill
4 C O N C L U S I O N
This study revealed that anthill, a naturally occurring material, could be
used as a low-cost adsorbent to remove Pb2+ and Zn2+ from aqueous
solution. The adsorption capacity of the cations from aqueous solution
descended in order of Pb2+ > Zn2+. The maximum removal percent-
age of the heavy metal ions was obtained at an optimum pH of 5. The
applicability of 2- and 3-parameter isotherm models for the adsorption
of heavy metals onto activated anthill was also discussed in detail. The
equilibrium adsorption isotherm study revealed that the isotherm data
fitted very well to the 3-parameter Radke–Prausnitz model.
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A U T H O R S’B I O G R A P H I E S
Adeyinka Sikiru Yusuff obtained his PhD from the Federal Univer-
sity of Technology, Minna, Nigeria, in 2017. He is a senior lecturer at
the Department of Chemical & Petroleum Engineering, Afe Babalola
University, Ado-Ekiti, Nigeria. His areas of research interests are cen-
tered on catalysis, renewable energy, separation process, and environ-
mental technologies.
Idowu Iyabo Olateju holds an MEng in chemical engineering from
the University of Lagos, Akoka Lagos, Nigeria. She is a lecturer at the
Department of Chemical & Petroleum Engineering, Afe Babalola Uni-
versity, Ado-Ekiti, Nigeria. Her areas of research interests are focused
on environmental management, biochemical engineering, and process
development.
How to cite this article: Yusuff AS, Olateju II. Experimental
investigation of adsorption capacity of anthill in the removal
of heavy metals from aqueous solution. Environ Qual Manage.
2018;27:53–59. https://doi.org/10.1002/tqem.21536
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