Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct.

2019 180-190

Journal of ChemResearch Volume 1, No. 2, Oct. 2019

Biosorption of Mercury (II) ions, Congo red dye and their binary mixtures from aqueous
solution using mango leaf powder (Magnifera indica) as adsorbent
Adelaja O. A.
Department of Chemistry, Federal University of Technology, P.M.B 704, Akure, Ondo State, Nigeria.

ABSTRACT
Non-pulverized biosorbent was obtained from the leaves of Mango tree (Magnifera indica).The
biosorbent was characterized using Fourier Transform Infrared spectrometry to elucidate the
functional groups present in the resultant powder. Experimental parameters such as pH, contact
time, adsorbent dosage and initial concentration were investigated. The maximum removal
efficiency of Congo red was 66.52% at pH 4, mercury was 95% at pH 8 and the binary mixture
at pH 5 was 72.33%. The experimental data better fit the Langmuir isotherm model for binary
mixture adsorption with a correlation coefficient, R2 of 0.9662 while Freundlich isotherm fitted
better for individual systems with R2 of 0.9265 for Congo red and 0.863 for mercury. The kinetic
data from this study fitted well with the pseudo-second order model, and adsorption profiles
derived based on the pseudo-second order kinetic model showed good agreement with the
experimental data. This study revealed the great potential of mango leaves in effective removal
of mercury, Congo red and their binary mixture from wastewater.
Keywords: Biosorbent, mango leaf, Congo red, binary mixture, kinetic data

1.0 Introduction pollution happens to be the most

The global increase in technological
advancement has led to release of harmful
pollutants into the environment. These
pollutants sometimes are released in very
high proportions making the environment
unsafe for mankind. Some of them which
are gaseous in nature diffuse into the
atmosphere and are the major cause of air
pollution; some are discharged into water
bodies leading to water pollution, while
others constitute nuisance to the
environment and cause land pollution. Water
180
predominant as water serves a lot of purpose
ranging from domestic, municipal, to
industrial applications (Gray et al., 2018;
Zushi and Masunaga, 2011; Cheremisinoff,
2002). Water pollution has become an
inevitable situation in the world as man’s
activities generate a lot of waste which are
being discharged into water bodies during
industrial processing (Scheren et al., 2002;
Wang et al., 2008; Zheng et al., 2017). Most
of these wastes from industries such as
mining, paint, paper and pulp, dye and
textiles industries(Chen et al., 2017;
 Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct. 2019 180-190

Hasanbeigi and Price, 2015) and many into the environment. As a result, a lot of
others, contain a lot of organic and inorganic research has been carried out on water using
particulates which could be biodegradable or various methods and various agricultural
non-biodegradable. These particulates such waste have been used.
as dyes (acid, basic, disperse, direct,
mordant), heavy metals like mercury, Various agricultural wastes have been used
cadmium, copper, arsenic and lead as biosorbents. These include sugarcane
accumulate at higher levels making water bagasse, rice husk, corn stalks, pawpaw
unpleasant to sight and gives a deteriorating leaves, baobab, mango leaves, mango seeds,
effect (Akinsanya and Kuton, 2016; Taiwo banana peels, orange peels and many others.
et al., 2018). Therefore, this study aimed at investigating
the removal of mercury, Congo Red dye and
Mercury as a heavy metal is toxic, and can their binary mixtures using mango leaves
recycle itself through the atmosphere, water, powder. The effect of solution pH, contact
and soil in various forms to different parts of time, initial concentration, adsorbent dose
the world (Junque et al., 2018; Saniewska et and temperature were investigated.
al., 2014; Fitzgerald and Lamborg, 2014). Adsorption kinetics and thermodynamics for
This can get bio-accumulated in aquatic biosorption mechanism was also proposed.
systems in form of highly toxic
methylmercury which can cause serious
health risks to humans. In view of this, there
is therefore a need to monitor and regulate 2.0 Materials and methods
its discharge into water bodies. Similarly,
wastewater with dyes affects the colour of 2.1 Preparation of Adsorbent
the water and restricts the penetration of
Mango leaves used in the study were gotten
sunlight thereby reducing photosynthetic
from Federal University of Technology,
activities of phytoplankton (Raturi and
Akure, (FUTA), Obakerere environs within
Fepuleai, 2010). Most synthetic dyes are
FUTA campus, Akure, Ondo State (as
carcinogenic and mutagenic (Chequer et al.,
shown in plates A, B and C). Mango leaves
2015). An example is the Congo red (CR),
were harvested for selective sequestration of
the sodium salt of benzidinediazobis-1-
Hg (II) ion and Congo Red dyes from
naphthylamine-4-sulfonic acid. It is a
aqueous medium. Mature mango leaves
benzidine-based azo dye and was selected in
were collected and washed thoroughly first
this study as a model anionic dye due to its
with tap water to wash off debris, with 0.4
high solubility in aqueous solution and its
M Hydrochloric acid solution (to remove
persistence once it is discharged into natural
metals) and then rinsed with deionized water
environment (Afkhami and Moosavi, 2010;
to remove dust and any adhering particles.
Ahmad and Kumar, 2010). It mainly occur
The leaves were air-dried for five days and
in the effluents discharged from textile,
then oven-dried at 80°C for 2 h until it
paper, printing and leather industries (Zheng
became crispy. The dried leaves were
et al., 2018). While dyeing, some of it ends
crushed and pulverize during a rotary
up in wastewater as a result of industrial
blender until a fine blend was obtained. The
discharge. It act as skin, eye and
resultant powder was sieved using 250µm
gastrointestinal irritant and is stable to
mesh size and stored in an airtight container
biological degradation (Fathima et al.,
for further analysis.
2018). It is therefore needed to be removed
from industrial effluents before discharge

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 Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct. 2019 180-190
A 60 ppm CR dye for CR determination or
B
C any time t concentration of metal/dye in
Plates: A, B and C of raw, dried and pulverized
mango leaves.
2.2 Preparation of Mercury Stock Solution
A 2000 mg/L Mercury (II) Chloride and 2000
mg/L stock solutions of Congo Red (CR) were
both prepared by dissolving 1g in 500 mL
distilled water. Appropriate dilutions of the
stock solution were carried out in order to
obtain the desired concentrations (ranging from
182
0- 150 ppm) of both Hg(II) and CR solutions
used in the study.
2.3 Batch adsorption studies
Adsorption studies were carried out as batch
experiments. This was done by weighing 0.1g
of the adsorbent unto different Erlenmeyer
flask containing either 50ml of 60 ppm Hg(II)
solution for Mercury determination, 50ml of
addition of 50ml of CR and Hg(II) to make
binary mixtures for Mercury and Congo red
determination. The content was agitated on an
orbital shaker of 100 rpm for 2 h. The samples
were withdrawn at appropriate time intervals
and filtered through Whatman filter paper
no.42. The supernatant was refrigerated in the
refrigerator (Midea HD-276F) until the metal
and dye analysis were done. The effect of pH
was investigated on pH range of 4 to 9 and
adjusted by adding dilute aqueous solution of
NaOH and HCl (0.1M). The adsorption
experiments were also used to determine the
equilibrium time, optimum pH, temperature
and dosage of the adsorbent for maximum
adsorption following similar procedure
described above. The metal/dye adsorbed (mg)
per unit mass of adsorbent was obtained using
equation 1:
Qt=(C0-Ct)V/m (1)
Where Qt is the amount of metal/dye adsorbed
at time t(mg/g); C0 and Ct are the initial and at
aqueous solution, respectively; V is the volume
of the solution (L); and m is the mass of the
adsorbent (g).
3.0 Results and Discussion
3.1 Characterization of adsorbent
The mango leaves powder used as adsorbent
was characterized to determine the functional
groups present using Fourier transform infrared
(FT-IR) spectroscopy. The spectrum was
 Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct. 2019 180-190
obtained with resolution range of 500–4000
cm-1. The broad and intense peak at 3408.33
cm-1and 3360.11cm-1 was attributed to the
stretching of O-H group due to inter and intra-
molecular hydrogen bonding of large
macromolecules of alcohols or phenols in
pectin, hemicelluloses, cellulose and lignin
(Arslanoglu et al., 2008). The peak observed at
2920.32cm-1and 2850.88cm-1was associated
with the of C-H stretch of methyl, methylene
and methoxy groups (Feng et al., 2008). The
band at 1720.56 was associated with C=O
bonds of the aldehyde group in lignin. The
peak at 1620.26 relates to C=C stretch (Fig. 1).
removal efficiency (%)
wavelength
Figure 1: FTIR Spectra of Raw Mango Leaf Powder
3.2 Effect of pH
The effect of pH on the adsorption of
Hg(II)ions, CR dye and Mercury-Congo (MC)
onto mango leaves was evaluated using 60
mg/L of their solutions respectively in the pH
range of 4 to 9 and the result is shown in
Figure 2. The adsorption of CR was highest at
pH 4 with a removal efficiency of 66.52%. The
uptake decreased rapidly to 42.64% at pH 5 to
37.91% at pH 6 and then an increase in uptake
occurs at pH 7 to 48.05%. The adsorption
efficiency reduced greatly between pH of 8 and
9 to 11.11%. CR being an anionic dye has
negative charges which will bind to the
positive sites on the adsorbent reluctantly at
high pH due to electrostatic repulsion. This
183
may be the reason why CR had maximum
adsorption capacity at pH 4 and on increasing
the pH, the number of negatively charged sites
increases and the number of positively charged
sites decreases. In addition, lower adsorption of
CR at pH 8 and 9 may be due to an abundance
of hydroxyl ions which competes with the dye
anions for the adsorption sites. Similar
observations were reported by Yu and Ya-juan
(2008).
80
60
congo
40 red
only
20
0
0 5
pH 10
Figure 2: Effect of pH on removal of Mercury, Congo
red and their binary mixtures by raw mango leaf
powder.
The adsorption efficiency of mercury increased
from 76.19% at pH 4 to 92.85% at pH 5 and
decreased consistently to 76.19% between pH
6 and 7, then increases to 95% at pH 8 and
90.43% at pH 9. The maximum adsorption
occurred at pH 8. The low adsorption at lower
pH values may be due to the predominance of
HgCl2 (Hg2+) and there is high concentration of
H+ resulting to less available sites for Hg2+ due
to the protonation of the surface functional
groups of the adsorbent (Yu and Ya-juan,
2008). However, an increase in removal
efficiency of Hg(II) ions at pH 8 may be due to
the presence of Hg(Cl)OH and Hg(OH)2
species, which are considered easier to be
adsorbed than HgCl2. Also, increase in the
degree of dissociation of carboxylic acid
groups results in an increase in the adsorption
of mercury ions (Yu and Ya-juan, 2008;
Anagnostopoulos et al., 2012). The removal of
 Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct. 2019 180-190
Mercury-Congo Red mixture (MC)
simultaneously using mango leaves powder
had maximum removal efficiency of 72.33% at
pH 5 and decreases with increasing pH. The
low removal could be attributed to competition
for the anionic groups between the CR
molecules and the amine groups on the mango
leaf powder.
3.3 Effect of contact time
The adsorption efficiency of Hg(II) ions
increased with increasing time from 30 min to
90 min (from 35-45% Hg removal) which
seems to be time of maximum adsorption and
then decreases at 120 min as shown in Figure
3. This was probably as a result of many active
sites available at the start of the experiment;
and as the sorption process proceeds, the free
binding sites became occupied causing a
slower biosorption rate until it approaches
equilibrium at 90 min due to the saturation of
active sites with Hg(II) ions (Al-Rmalli, et al.,
2008; Taha, et al., 2017). The observed fast
biosorption rate may also be associated with
biosorption of metal involving non energy-
mediated reactions, where metal removal from
solutions is purely due to physicochemical
interactions between the biomass and the metal
solution. The increased in adsorption of CR at
30 min of contact with the mango leaves
powder may be as a result of availability of a
larger surface area of the mango leaf powder at
the beginning for the adsorption of dye ions
(Thomas, 2016). The adsorption efficiency of
the mango leaf to remove both Hg(II) ions and
CR dye effectively also increased between the
first 30 min of contact time and adsorption
becomes slower at higher contact time.
184
70
60
removal efficiency (%)
50 congo red
40
30
mercury
20
mercury-
10 congo
0
30 60 90 120 150
time (mins)
Figure 3: Effect of contact time on adsorption of
Mercury, Congo red and their binary mixtures onto
mango leaf powder.
3.4 Effect of adsorbent dose
The removal of mercury from aqueous solution
increased up to an adsorbent dose of 0.05g,
after which it decreases on increasing the
adsorbent dose. This may be due to the large
adsorbent amount which effectively reduces
the unsaturation of the adsorption sites.
Correspondingly, the number of such sites per
unit mass comes down, resulting in
comparatively less adsorption at higher
adsorbent amount. The higher adsorbent
dosage also creates particle aggregation,
resulting in a decrease in the total surface area
and increase in the diffusion path length, which
lead to decrease in the amount of adsorbed Hg
(II) ions per unit mass of adsorbent (Gupta and
Bhattacharyya, 2008; Viera et al., 2010). For
CR, there is an increase in adsorption with
increasing adsorbent dosage until it reached a
maximum at 0.20g where the removal
efficiency decreased. The removal of MC
increased greatly to 73.81% unlike the single
system where it was 57.14% for mercury and
24.86% for CR.
 Adelaja O. A. jocr.futa.edu.ng. Vol. 1, No 2, Oct. 2019 180-190

80.0 70
70.0
removal efficiency(%)

60
60.0

removal efficiency (%)

50.0 50
congo red
40.0
40 congo
30.0 mercury
mercury-congo 30 mercury
20.0
10.0 mercury-congo
20
0.0
0 0.1 0.2 0.3 10
adsorbent dose(g)
0
Figure 4: Effect of adsorbent dose on removal of
mercury(II)ions, Congo red and mercury-Congo red 30 60 90 120
concentration (ppm)
mix on Mango leaf powder.
Figure 5: Effect of initial concentration on adsorption
of mercury, congo red and their binary mixtures on
3.5 Effect of Initial concentration
raw Mango leaf powder.
The adsorption of mercury increased with
increase in concentration in a single pollutant
system. The maximum adsorption was obtained
at 120 mg/L. The effect of initial metal
concentration in the range of 30 to 120 mg/L
on adsorption is shown in figure 5. It showed
that the removal of metal was dependent on the
concentration of metal as the increase in the 3.5 Adsorption Isotherm
initial concentration increased the amount Langmuir isotherm
removed up to 50 mg/L for mercury and
decreases at higher concentrations. This The plot of Ce/qe against Ce gave a straight line
1
observed trend may be due to the increase in with slope of and intercept of 𝑞 𝐾 . Figure
𝑚 𝐿
the driving force offered by the concentration
6 showed the Langmuir plots of Hg(II) ions,
gradient as reported (Gang et al, 2010). The
CR and their binary mixture adsorption by
adsorption of CR increases till the
mango leaf with a correlation coefficient, R2,
concentration of 90 mg/L and then begin to
of 0.762,0.921,0.966 for Hg(II), CR and MC
decrease. In the binary component system,
respectively. R2 for MC was closer to unity
removal efficiency of both dye and metal
thus indicating that the data do conform well to
decreases with increase in concentration.
the Langmuir isotherm model. According to
Decrease in removal efficiency as notably
the Langmuir equation, the maximum uptake
observed in the binary system might be due to
capacity was 23.70 mg/g, 23.09 mg/g and
the competitive effect of two pollutant
20.24 mg/g for Hg(II), CR and MC
molecules for the active site on the absorbent
respectively. The Langmuir parameters were
surface. A similar observation was reported by
also used to predict the affinity of the mango
Fernandez et al. (2010) using Cupressus
leaf powder surfaces towards the Hg(II) ions,
sempervirens cone chips for the biosorption of
CR and MC.
Methyl Blue and rhodamine B in binary and
single systems.

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y = 0.2812x + 0.6868
2.500
7 y = 0.0422x + 1.6438 y = 1.7003x - 0.1532 R² = 0.9224
y = 0.0494x + 0.8104y = 0.0433x + 1.7904
R² = 0.9662
R² = 0.7619 2.000 R² = 0.9265
6 R² = 0.921
1.500

log ce
5 mercury
1.000
4 y = 0.4894x + 0.2793 congo red
ce/qe

mercury
0.500 R² = 0.863
3 congo red mercury-congo
0.000
2 mercury-congo 0.000 1.000 2.000 3.000
1 log qe

0
Figure 7: Freundlich isotherm plot for adsorption of
0.000 20.000 40.000 60.000 80.000 100.000
Hg(II) ions, Congo red and their binary mixture on
ce Mango leaf powder
Figure 6: Langmuir isotherm plot for the sorption of
Hg(II) ions, BET Adsorption isotherm
Congo red dye and their binary mixtures on mango
leaf powder The BET plot for biosorption of Hg(II) ions,
CR and MC onto Mango leaf, with their
correlation coefficients of 0.8398, 0.9258 and
0.8515 respectively are shown in Figure 8. The
Freundlich value of qm and Kb obtained for Hg(II) ions,
CR, and their binary mixture was found to be
The plot of log qe against log Ce gave a straight (0.0046 and -3.148), (0.0107 and -0.9109) and
line. Figure 7 shows the Freundlich isotherm (0.0046 and -2.107) respectively.
plot of Hg(II) ions, CR and MC adsorption
onto mango leaves, with a correlation y = 93.206x - 29.998
coefficient of 0.863, 0.9265 and 0.9224 50.0 R² = 0.8515
y = 195.57x - 102.34
respectively. The values of KF and n obtained 45.0
R² = 0.9258
from the plots for mercury, CR and MC were 40.0
y = 147.61x - 68.72
(1.902 and 2.04), (1.4229 and 1.000) and 35.0 R² = 0.8398
ce/(cs-ce)qe

30.0
(1.9024 and 3.556) respectively. The “n” value mercury
25.0
of Freundlich equation could indicate the congo red
20.0
favorability of the adsorption process. It is 15.0 mercury-congo
usually stated that values of “n” in the range of 10.0
2 to 10 is good, 1 to 2 as moderately good and 5.0
less than 1 as poor sorption characteristics 0.0
(Chen et al., 2017). 0.000 0.200 0.400 0.600 0.800
ce/cs

Figure 8: BET isotherm showing adsorption of

Mercury, Congo red and Mercury-Congo onto raw
mango leaf powder.

3.6 Adsorption kinetic studies

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The study of adsorption kinetics in wastewater

5.0
treatment is relevant as it provides good insight y = -0.016x + 4.5933
4.5 R² = 0.891
into the reaction pathways, the mechanism of
adsorption reaction, and also give detailed 4.0
information on the adsorbate uptake rate, 3.5
which in turn control the residence time of 3.0

ln(qe-qt)
adsorbate uptake at the solid-solution interface. 2.5
The kinetics data obtained from adsorption of 2.0
y = -0.0168x + 3.7524
y = -0.0262x + 3.927R² = 0.8563
Hg(II) ions, CR and MC onto mango leaf was 1.5 R² = 0.9811
mercury
studied by using three kinetic models, which
1.0
are the pseudo-first order kinetic model, congo red
0.5
pseudo-second order kinetic model and the mercury-congo
intra-particle model. The best fit model was 0.0
0 10 20 30 40
selected based on the linear regression t(mins)
correlation coefficient (R2), which is a measure Figure 9: Pseudo-first order kinetic plot for
of how well the predicted values from a adsorption of Hg(II) ions, Congo red in single and
forecast model match with the experimental binary mixture on mango leaf powder.
data.
Figure 9 shows the linear plots of pseudo-first
order where log(qe-qt) against t at initial Hg (II) Table 1: Pseudo-first order kinetic plot for
ions, CR and MC concentration of 120 mg/L. adsorption of Hg(II) ions, Congo red in single and
binary mixture on mango leaf powder
The k1 and qe values were determined from the
slope and intercept of the linear plots R2 qe(mg/g) qe(mg/g) K1(g/
respectively. Mercury had the highest R2 value (calculated) (exptal) mgmin)
Mercury 0.9811 50.75 72.68 0.0262
but had a low qe value compare to that of the
Congo red 0.891 98.81 84.34 0.0160
experimental data obtained. This suggested a MC 0.8563 42.62 42.38 0.0168
poor fit between the kinetics data and the
pseudo-first order model [Ong-pick, 2011]. It
was observed from Figure 9 and Table 1 that 2.5
the first-order model failed to provide a
y = 0.0449x + 0.7278
realistic estimate of qe of adsorbed Hg (II) ion 2.0 R² = 0.8477
y = 0.0287x - 0.084
R² = 0.9846
onto mango leaves, because the experimental
values of qe were higher than the calculated qe.
This showed that the pseudo-first order kinetic 1.5
congo red
t/qt

model for the adsorption of Hg (II) ions onto mercury

mango leaf powder is not appropriate to 1.0 mercury-congo
y = 0.0186x + 0.0658
describe the entire process and is not a first- R² = 0.9988
order reaction.
0.5

0.0
0 10 20
t(mins) 30 40
Figure 10: Pseudo-second order of adsorption of
Mercury, Congo red and their binary mixtures on
mango leaf powder

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Table 2: Pseudo-second order kinetic plot for
adsorption of Hg(II) ions, Congo red in single and
binary mixture on mango leaf powder
R2 qe(mg/g) qe(mg/g) K2
(calculated) (exptal) (min-1)
Mercury 0.9988 53.76 72.68 0.0053
Congo red 0.8477 22.81 84.34 0.0028
MC 0.9846 11.90 42.38 0.2458
The values of qe and h were calculated from the
slope and intercept of the plots in Figure 10
respectively. Table 2 gives the values of k2,
experimental and calculated values of qe, as
well as the R2 values for the pseudo-second
order plots. It was observed that the three plots
were linear with different initial concentration
and shows R2 values close to 1. This indicated
that the kinetics data fitted perfectly well with
the pseudo-second order model.
From Table 2, it was observed that the values
of h for Hg(II)ion was 15.19 mg/mg min at 120
mg/L initial concentration of Hg(II) ions. This
was because the higher the initial concentration
of Hg(II) ion, the higher the chances of
collision with the binding sites of adsorbent
and hence, leads to a higher initial adsorption
rate (Zushi et al., 2011).
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4.0 Conclusion
The present study has shown the effectiveness
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