Aden Uga 2019
Aden Uga 2019
Aden Uga 2019
A R T I C LE I N FO A B S T R A C T
Keywords: Among the contaminants that are frequently associated with industrial wastewaters, potentially toxic metals are
Wastewater of great health concern because they are non-biodegradable and can be transformed by biochemical processes to
Agricultural waste more poisonous metal-organic complexes. Thus, safe and adequate disposal of wastewater containing these
Potentially toxic metals metals into the environment remains a front-burner challenge. This study investigated metal ions removal from
Kinetics
wastewaters using adsorbents generated from the Spent Seedcake of Calophyllum inophyllum (SSCI) as an al-
Adsorption isotherms
Thermodynamics
ternative low-cost adsorbent. Batch adsorption process was employed to demonstrate the adsorption capacity for
the multi-component removal of Pb(II), Cd(II) and Zn(II) at optimized experimental conditions. Carbonization
and microwaving of the biosorbent produced an optimal performance for the uptake of the metals at solution pH
of 9, temperature of 30 °C, dosage, 10 g/L and 60 min equilibrium time. The maximum adsorption capacities of
the biosorbent were 52.63, 51.28 and 17.99 mg/g for Pb2+, Cd2+and Zn2+ respectively. The adsorption kinetics
of the metals unto the biosorbent was adequately described by a pseudo-second-order kinetic model with po-
sitive enthalpy (ΔH) indicating the endothermic nature of the adsorption process while the negative values of the
Gibbs free energy (ΔG) confirmed the spontaneity of the adsorption process for all the metals studied.The ef-
fectiveness of the biosorbent was tested with real wastewater samples and a removal of the metals between
55–71% was achieved.
⁎
Corresponding author.
E-mail address: adenugaa@oauife.edu.ng (A.A. Adenuga).
https://doi.org/10.1016/j.jece.2019.103317
Received 6 June 2019; Received in revised form 20 July 2019; Accepted 23 July 2019
Available online 26 July 2019
2213-3437/ © 2019 Elsevier Ltd. All rights reserved.
A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
compounds like chromium and cadmium compounds [6]. 2. Material and methods
Over the years, the unethical discharge of high volumes of waste-
water laden with large amounts of potentially toxic metals into water 2.1. Reagents used, biosorbent preparation and characterization
bodies has generated austere health and environmental concerns with
the outcry on possible epidemic outcomes across the globe [1]. Yet, The analytical grade chemicals and reagents used were obtained
total stoppage of such illicit activities by industries is far from being from Sigma-Aldrich and BDH and were used without further purifica-
achieved. The problem of discharge of untreated or inadequately tion. The SSCI was obtained as waste, after oil extraction from a re-
treated wastewater into the environment is even more pronounced in search laboratory at the Obafemi Awolowo University, Ile-Ife, Nigeria.
most developing nations of the world in spite of existing environmental The spent cake was washed with hot water, filtered and thoroughly
regulations, demanding an improved quality of industrial effluents. This rinsed with warm distilled water to remove residual oil. It was then
is partly because of the high cost of conventional treatment techniques oven dried at 105 °C until constant weight of 207.23 ± 0.47 g was
[7–9] and low or no enforcement of the existing environmental laws. attained. A portion of the oven-dried spent seedcake was crushed and
Complete ignorance or low awareness of the adverse impact of sieved through a mesh of 500 μm. This served as the unmodified ad-
wastewaters enriched in potentially toxic metals, in many communities, sorbent. Other portions of the spent cake were carbonized in a muffle
is a major obstacle to curbing the exposure of humans and animals. furnace (50 Hz, 9 Amps, 220/240 V, England). Carbonization was car-
Several farmers depend on water bodies into which untreated industrial ried out by heating at 20 °C /min from room temperature until 500 °C
effluents are being discharged for their farming activities, such as irri- and then held for 45 min. The samples were then left to cool to room
gation, fish farming and a source of water for their animals. Most of the temperature in a desiccator. The carbonized samples were then crushed
toxic metals, for example, cadmium, arsenic, lead, and mercury, do not and sieved through a pore size of 500 μm and stored in an airtight
perform any physiological and metabolic functions in man and animals; plastic container pending further treatments or usage. Portions of the
rather they cause major adverse health effects. Certainly, few of the raw and charred samples were subjected to further modification by
metals are essential and serve as nutrients to plants and animals by either one method or a combination of methods. A portion of each of
virtue of their physiological and metabolic functions, such metals in- raw and charred spent seedcake samples was soaked in 0.2 M sulphuric
clude selenium, zinc, iron, and copper. However, they are needed in acid for 48 h for acid modification. The samples were filtered, thor-
trace amounts and will always constitute a danger to man and en- oughly washed with distilled water until the pH was neutral and dried
vironment at elevated concentrations especially when their permissible overnight at 105 °C. The acid-modified biosorbent materials were
limits are exceeded [10–,11,12]. The impact of ingested or contacted stored in an airtight plastic container pending further use. The micro-
potentially toxic metals on humans can be classified as toxic (acute, wave modification was carried out by placing dry samples in a micro-
chronic or sub-chronic), carcinogenic, neurotoxic, mutagenic or ter- wave oven with an input power of 400 W and 4 min irradiation time.
atogenic [13]. The ionic forms of these metals constitute the most dif- These were done to investigate the modification(s) best suited for op-
ficult environmental menace since they do not succumb to natural de- timum performance of the biosorbent. For characterization, the surface
gradation or transformation to less harmful form but are easily morphologies of the unmodified, the selected modified adsorbents
absorbed by plants and aquatic animals for reason of their high solu- (before and after adsorption process) were determined with Scanning
bility. Humans are subjected to the higher dose of these metals by Electron Microscopy (SEM) (TESCAN, Vega 3 XMU, Czech Republic)
means of biomagnifications as we move up the food chain and due to and the surface elemental compositions determined with Energy-
their bioaccumulation ability, they are accumulated in the human body Disperse X-ray Spectrometer (EDS) (TESCAN, Czech Republic) that is
leading to diverse health hazards. attached to the SEM. Fourier Transform Infra Red spectroscopic ana-
A variety of conventional technologies for wastewater treatment are lyses were performed using Shimadzu FTIR (Model IR 8400S, USA)
available with different degrees of success to control and minimize the
amount of pollutants being released into the environment, especially 2.2. Preparation of adsorbates and analysis
water bodies; such as ion exchange, chemical precipitation, electro-
dialysis, membrane filtration, oxidation, reverse osmosis, flocculation, Lead, Cadmium and Zinc solutions of desired concentrations were
solvent extraction, evaporation, phytoremediation and activated carbon prepared by dilution of a stock solution containing the mixture of the
adsorption [14–19]. Nevertheless, the inadequacies of the majority of metal ions at a concentration of 1000 mg/L each. The stock solution
these techniques are high running and maintenance costs, production of was prepared by dissolving calculated amounts of the nitrate salt of the
toxic sludge and complex processes involved in the treatment [20]. metals (Cd(NO3)2, Pb(NO3)2 and Zn(NO3)2) in distilled water. The in-
Relatively, adsorption process has demonstrated to be a better sub- itial concentration of the metal ions in solution and the residual metals
stitute in water and wastewater treatment because of handiness, ease of in solution after adsorption equilibrium was analyzed using Flame
the process and simplicity of design design ([20–23]. The high ad- Atomic Absorption Spectrophotometer (FAAS) (AA990 F, PG
sorption capacity of the low-cost by-products from agricultural sector as Instrument Ltd, United Kingdom). Air–acetylene system was used for all
adsorbents have been tested and found preferable and very attractive determinations. ISO 17,025 certified metal reference standards used
alternative adsorption materials [24,9,25,4,26,17]. Therefore, utiliza- were obtained from MRS Scientific Ltd, Wickford, Essex, UK.
tion of agricultural wastes as adsorbent proffers exceedingly valuable
technological means of handling potentially toxic metals pollution and 2.3. Experimental design
at the same time contributes to waste minimization and management,
with minimum investment required [27,28,17]. This field is therefore, a Batch adsorption process was employed throughout the study. The
means to the end of lingering wastewater problems in the developing first stage of the study dealt with the optimization of the conditions
countries to alleviate or at least, reduce the impacts of industrial was- under which the adsorbent will demonstrate the best adsorption capa-
tewater pollution. For the well-being of man and his environment, it is city for the removal of the metals. Biosorbent was allowed to interact
very important that more agricultural wastes as low-cost materials are with the solution of the selected metals, Pb, Cd, and Zn, simultaneously
sourced to help industries in the treatment of their wastewaters for while conditions; pH, initial concentration of adsorbates, dosage of the
appropriate control of heavy metal releases into the environment. This biosorbent, temperature and contact time were varied. The combina-
study explores the possibility of the use of SSCI, an industrial waste, as a tion of the optimum of each condition evaluated was chosen for further
viable and sustainable low-cost biosorbent for simultaneous adsorption work. The biosorbent was then applied to two types of real water
of Pb(II), Cd(II) and Zn(II) from wastewaters. samples: (1), Effluents from a metal smelting company - representing
industrial wastewater and (2), domestic waste contaminated stream.
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
2.4. Influence of operating parameters and equilibrium studies intra-particle diffusion rate constant kp. were calculated from the data
obtained.
Initial screening of the adsorbents was conducted by contacting Thermodynamic studies help us to understand the feasibility and
0.5 g of the biosorbent types with 50 mL of metal ions solution at a spontaneous nature of the biosorption. The Changes in Gibbs free en-
concentration of 25 mg/L per metal and agitated by sonication ergy (ΔG), enthalpy (ΔH) and entropy (ΔS), are used in the evaluating
(Ultrawave, 100 W, 50–60 Hz) for 120 min. Then biosorbent was se- the thermodynamic properties of biosorption process. These parameters
parated from the solution by filtration, and the filtrate analyzed with were calculated using the following expressions:
FAAS. Results obtained were used as a guide in the selection of the most
CA
appropriate modification for the biosorbent, based on effectiveness. The KC =
CS (5)
effect of pH on the adsorption capacity was studied in the pH range of
3.0–9.0, which is the range found in most industries discharged was-
ΔS ΔH
tewaters depending on the type of industry [7]. The dosage dependence ln K C = −
R RT (6)
of the metal uptake was studied in the range of 2–22 mg/L while the
influence of initial metal ion concentration was studied in the con- ΔG = ΔH − TΔS (7)
centration range of 0–200 mg/L. The dependency of the adsorption
process on temperature was evaluated at different temperatures of 20, KC represents the distribution coefficient, CA, the quantity of ad-
30, 40 and 50 °C. Langmuir and Freundlich's isotherms were used to sorbates adsorbed, CS, concentration of adsorbates in solution at equi-
verify the results of these equilibrium studies. The equilibrium ad- librium, R, the gas constant with a value of 8.314 J/mol K and T,
sorption capacity of the biosorbent, qe, representing the amount of temperature in kelvin [32,33]. The effect of temperature on the bio-
metal ions adsorbed by the biosorbent (mg/g) at equilibrium was cal- sorption process was studiedby varying temperature from 20 to 50 °C,
culated using Eq. 1 with time, keeping other parameters such as biosorbentdosage, ad-
sorbates concentration, and pH, constant.
( C0 − Ce )
qe = V
M (1)
2.6. Adsorption isotherms
where Co = initial concentration of metal ion in solution (mg/L);
Ce = concentration of the metal ion in solution at equilibrium (mg/ To understand the mechanism of the biosorption process and de-
L); termine the maximum biosorption capacity of the biosorbent, the
V = volume of solution (L); Langmuir [34] and Freundlich [35] isotherms, which are the most
M = mass of adsorbent (g). commonly used models, were applied on the equilibrium data obtained
experimentally. The linearized form of the Langmuir equation is re-
2.5. Kinetic and thermodynamicstudies of the biosorption process presented as:
Ce 1 C
Using different models that includes pseudo-first order, pseudo- = + e
qe KL Q0 Q0 (8)
second order and intraparticle diffusion the dependence of the ad-
sorption data on time was evaluated. where qe = quantity ofheavy metal adsorbed on the biosorbent (mg/g);
The first order parameters were obtained using the linearized Ce = equilibrium concentration of metal (mg/L) in the solution;
Lagergren’s first order rate equation [29], given as: Q0= maximum adsorption capacity of the biosorbent (mg/g);
ln (qe − qt ) = ln qe − k1 t (2) KL= equilibrium constant related to the energy of biosorption,
which reflects quantitatively the affinity of the binding sites for the
In which qt and qe are the quantities (mg/g) of metal ion adsorbed at metals (L/mg) (Mahmoodi [36]. When Ce/qe is plotted against Ce a
a specified time, t, and equilibrium time respectively, and k1in min−1 is straight line is obtained whose slope equals 1/Q0 and intercept equals
the rate constant, which can be obtained from the slope of the plot of ln KL.
(qe – qt) against t. The linearized form of the Freundlich isotherm model is given as:
The linearized form of pseudo-second order equation [30] was used
to obtain the second order parameters, given as: 1
log qe = log kf + log Ce
n (9)
t 1 t
= +
qt k2 qe2 qe (3) kf and1/n are Freundlich isotherm constants related to adsorption ca-
pacity of the biosorbent (L/g) and intensity of adsorption, respectively.
The equilibrium constant of the process k2 (g mg−1 min−1),can be The plots of log qe against log Ce gives a straight line whose slope equals
calculated from the intercept of the linear plot of t/qt against t. 1/n with an intercept corresponding to log kf
Intra-particle diffusion model as given by Furusawa and Smith [31]
is as follows:
3. Results and discussion
1
qt = kp t 2 + I (4)
3.1. Influence of modification on the performance of biosorbent
−1 -1/2
Where kp(mgg min ) represents the intra-particle diffusion rate
constant which can be calculate from the slope of a plot of qt against t1/ Table 1 shows the results of the percent of metals adsorbed (%) by
2
,and I, the intercept (mg g−1) the various biosorbent types evaluated. From the results, there is a clear
For the kinetic studies, 50 mL each of simulated wastewater solution indication that modification did enhance the performance of the bio-
containing the mixture of the metals at concentrations of 50, 100, 150 sorbent at different degree depending on the modification type. Al-
and 200 mg/L for each metal ion was contacted with 0.5 g of the ad- though, charring only marginally performed best for the uptake of Zn, a
sorbent at 30 °C. The mixture was shaken continuously and monitored combination of charring and microwaving performed best for the up-
at a time interval of 20 min over a period of 120 min. The solution was take of Cd(II), Pb(II) and Zn(II), and performed excellently well with Zn
then filtered and the residual metal ion concentration in the super- (II) when the metals were adsorbed concurrently in solution. Thus, a
natant solution was analysed using FAAS. The Lagergren’s pseudo-first- combination of charring and microwaving of the biosorbent was
order rate constant, k1, Ho’s pseudo-second-order rate constant, k2, and adopted as the appropriate modification for this work.
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
Table 1 a result of the metal adsorption unto the biomass. The results show that
Summary of the influence of modification on the performance of the biosorbent, chemical interactions took place on the adsorbent surface between the
presented as percent uptake (%): initial concentration of each metal −OH/-NH group and the metal ions [42,43].
ion = 25 mg/L; temperature = 30 °C; biosorbent dosage = 10 g/L; time
=120 min.
Treatment Cd Uptake (%) Pb Uptake (%) Zn Uptake (%) 3.3. Influence of pH on biosorption process
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
Fig. 1. Scanning electron micrographs (SEM) (a–c) and Energy dispersive X-ray (EDX) (d–f) of the biosorbent (a & d) unmodified, (b & e) modified (charred and
microwaved), (c & f) modified and loaded with adsorbates, and (g) FT-IR spectra of unmodified, unloaded modified and loaded modified biosorbents.
3.6. Influence of contact time and the initial concentration of adsorbates on 40 min and reaching maximum at 60 min. There were no significant
biosorption efficiency change in equilibrium state after 60 min hence, the optimum time for
adsorption to reach equilibrium was set at 60 min for further work. The
The impact of contact time of biosorbent with the adsorbates on the adsorption capacities of the biosorbentat 50, 100, 150 and 200 mg L−1
biosorption efficiency initial concentrations for each metal ion were found to be 4.96, 8.22,
for varied initial concentration of the adsorbates (Pb(II), Cd(II) and 10.07 and 10.86 mg g-1 respectively for Pb(II); 4.97, 8.06, 9.71 and
Zn(II)) is shownin Fig. 3a & b, temperature: 30 °C; pH 9; biosorbent 10.38 mg g-1 respectively for Cd(II); 4.96, 7.93, 8.90, and 9.25 mg g-1
dosage of 10 g/L. The results showed the adsorption capacity increasing respectively for Zn(II). The general increase in adsorption capacity
rapidly with contact time, up to 40 min, for all the different initial observed at higher concentration of metal ions is associated to a more
concentrations of all the three metals with only slight increase after effective interaction between sorbent active sites and adsorbates which
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
From the results obtained from fitting the experimental data of the
biosorption process into Langmuir and Freundlich isotherm models,
Figures S4& S5, respectively, it can be inferred by the virtue of the
values of correlation coefficients(Table 2b), that both models explained
the biosorption process adequately, but the Freundlich model better
explained the mechanism for the biosorption of Pb(II) and Cd(II) ions,
indicating a heterogeneous biosorptive process,while Langmuir model
better explained the mechanism for Zn(II) ion, indicating a homogenous
monolayer biosorptive process [53,54].Igwe &Abia, [55], showed that
the isotherm that best describes an adsorption process depends on
thepH of the solution and is specific for different fordifferent metals
Based on the Q0 values of the Langmuir model, the maximum
Fig. 2. Effects of pH (a): time =120 min, dosage = 10 g/L, conc. = 100 mg/L, seedcake biosorption capacity (mg/g) for the metals followed the order:
temp. = 30 °C; Adsorbent dosage (b): pH = 9, time =120 min, Pb > Cd > Zn. Comparing the maximum adsorption capacity of the
conc. = 100 mg/L, temp. = 30 °C; Temperature (c):pH = 9, dosage = 10 g/L, modified spent seedcake of C. inophyllum biochar studied in this work
time =60 min, conc. = 100 mg/L on the adsorption of Pb(II), Cd(II) and Zn(II) with some other biosorbents that have been reported in the literature
onto spent seedcake of C. inophyllum biochar. (Table 3), it is a testimony that the modified spent seedcake of C. in-
ophyllum biochar performed well for simultaneous adsorption of toxic
metal with little influence of the solution matrix.
3.9. Thermodynamics
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
Table 2
Kinetics, adsorption isotherms and thermodynamics data for the adsorption process.
(a). Pseudo-first order, Pseudo-second order and Intra-particle diffusion parameters for the adsorption of Pb(II), Cd(II), and Zn(II) onto spent seedcake of C. inophyllumbiochar at 30 °C
Pb 7.54 25.57 −0.1010 0.7462 7.87 0.0299 1.0000 0.2531 5.3445 0.9321
Cd 7.63 20.71 −0.0864 0.8888 8.30 0.0147 0.9930 0.4240 3.4708 0.8710
Zn 7.42 28.95 −0.0912 0.9256 8.58 0.0085 0.9962 0.2481 5.2945 0.8496
(b). summary of isotherm parameters for the sorption of Pb (II), Cd (II) and Zn (II) on the spent seedcake of C. inophyllum (biochar)
Langmuir Freundlich
2
Metal Q0(mg/g) KL (L/g) R kf 1/n R2
(c). Thermodynamic parameters for biosorption of Pb(II), Cd(II) and Zn(II) onto the spent seedcake of C. inophyllum
Table 3 saturation of the biosorbent active surface and also to matrix effect,
Comparison of the Maximum Adsorption Capacities of some Adsorbents with resulting in co-adsorption of interferences present in the wastewater
spent seedcake of C. inophyllum (biochar). [65]. The results revealed that the biosorbent is capable of remediating
Q0 (mg/g) metals in wastewater to permissible levels when the concentration is
within ≤ 25 mg/L and will also do well at higher concentrations.
Adsorbent material Pb Cd Zn Reference
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A.A. Adenuga, et al. Journal of Environmental Chemical Engineering 7 (2019) 103317
Appendix A. Supplementary data [27] W.W. Ngah, M.A.K.M. Hanafiah, Removal of heavy metal ions from wastewater by
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online version, at doi:https://doi.org/10.1016/j.jece.2019.103317. dustry’s wastewater using leca as an available adsorbent, Int. J. Environ. Sci.
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