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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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