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MN Removal by Electrocoagulation-Adsorption Kinetics
MN Removal by Electrocoagulation-Adsorption Kinetics
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The present study provides an electrocoagulation process for the removal of manganese (Mn) from water using magnesium as anode and galvanised
iron as cathode. The various operating parameters like effect of initial pH, current density, electrode configuration, inter-electrode distance,
coexisting ions and temperature on the removal efficiency of Mn were studied. The results showed that the maximum removal efficiency of 97.2%
at a pH of 7.0 was achieved at a current density 0.05 A/dm2 with an energy consumption of 1.151 kWhr/m3 . Thermodynamic parameters, including
the Gibbs free energy, enthalpy and entropy, indicated that the Mn adsorption of water on magnesium hydroxides was feasible, spontaneous
and endothermic. The experimental data were fitted with several adsorption isotherm models to describe the electrocoagulation process. The
adsorption of Mn preferably fitting the Langmuir adsorption isotherm suggests monolayer coverage of adsorbed molecules. In addition, the
adsorption kinetic studies showed that the electrocoagulation process was best described using the second-order kinetic model at the various
current densities.
M
anganese (Mn) is the second most abundant metal in
2006a, 2008, 2009; Ali and Gupta, 2007; Ali and Gupta, 2008;
nature (Dabeka et al., 2002). It is an essential metal for
Bedow et al., 2008; Gupta and Rastogi, 2008a; Gupta and Suhas,
the human system and many enzymes are activated by
2009; Vasudevan et al., 2010). Physical methods like ion exchange,
Mn. Mn has a variety of applications in ceramics, primary cells
reverse osmosis and electrodialysis have proven to be either too
(dry battery) and electrical coils. Mn is also used in alloying ele-
expensive or inefficient to remove Mn from water. At present,
ment of many alloys. It is present in the atmosphere as suspended
chemical treatments are not used due to disadvantages like high
particulates resulting from industrial emission, soil erosion, vol-
costs of maintenance, problems of sludge handling and its dis-
canic emissions and the burning of MMT-containing petrol (WHO,
posal and neutralisation of effluent (Melnik et al., 1999; Mollah
2004). The Mn contaminant in ground water affects the intelligent
et al., 2001; Mouedhen et al., 2008). Recent research has demon-
quotient (IQ) of children (Dabeka et al., 2002). The neuro-
strated that electrocoagulation offers an attractive alternative to
toxic disease like Parkinsonism is caused by the Mn over intake
above-mentioned traditional methods for treating water (Mollah
(Erikson et al., 2007). The prolonged over intake is potentially
et al., 2001). In this process, anodic dissolution of metal electrode
affect the central nervous system and lungs. These Mn contam-
takes place with the evolution of hydrogen gas at the cathode
inants in the ground water cause a disease, called manganism
and also causes diseases of disturbed speech called prognosis,
also cause bronchitis and pneumonia (USEPA report). The World ∗ Author to whom correspondence may be addressed.
Health Organisation (WHO) prescribed the permissible limit for E-mail address: vasudevan65@gmail.com
the Mn in the ground water is 0.05 mg/L (WHO, 2004). Can. J. Chem. Eng. 91:448–458, 2013
The common methods for removing toxic metals from water © 2012 Canadian Society for Chemical Engineering
DOI 10.1002/cjce.21709
include electrodialysis, chemical coagulation, reverse osmosis, Published online 4 June 2012 in Wiley Online Library
co-precipitation, complexation, solvent extraction, ion exchange (wileyonlinelibrary.com).
| 448 | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | | VOLUME 91, MARCH 2013 |
(Mouedhen et al., 2008). Electrochemically generated metallic
ions from the anode can undergo hydrolysis to produce a series
of activated intermediated that are able to destabilise and adsorb
(Gupta et al., 1997a, 2006b, 2007; Gupta and Rastogi, 2008b) the
finely dispersed particles present in the water to be treated. The
adsorbed/destabilised particles then aggregate to form flocks as
outlined below:
(i) When iron/aluminum is used as the electrode, the reactions
are as follows:
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THEORY equilibrium curves. In this study, two adsorption isotherms, viz.,
Langmuir and Freundlich were applied to establish the relation-
Adsorption Kinetic Modelling ship between the amounts of Mn adsorbed onto the magnesium
The amount of generated coagulant (metal hydroxides) can be sto- hydroxides and its equilibrium concentration in the electrolyte
ichiometrically determined according to Faraday’s law. Since the containing Mn ions (Hamadi et al., 2001).
amount of coagulant can be estimated for a given time, the pollu-
tant removal can be modelled using an adsorption phenomenon. Freundlich Isotherm
In order to investigate the mechanisms of the adsorption process, The Freundlich adsorption isotherm model includes considera-
two different kinetic models, the first- and second-order Lagergren tions of surface heterogeneity and exponential distribution of the
models were applied to describe the kinetics of the Mn adsorp- active sites and their energies. The isotherm is adopted to describe
tion onto magnesium hydroxides. The best-fit model was selected reversible adsorption and is not restricted to monolayer formation.
according to the linear regression correlation coefficient values, This isotherm typically fits the experimental data over a wide
R2 (Johnson, 1990). range of concentrations. The linearised and logarithmic expres-
sion of the Freundlich model is (Agrawal and Sahu, 2006):
First-Order Lagergren Model
log qe = log kf + n log Ce (12)
The first-order Lagergren model is one of the most widely used
expressions describing the adsorption of solute from a solution.
where kf (mg/g) and n (dimensionless) are constants that account
The first-order Lagergren model is generally expressed as follows:
for all factors affecting the adsorption process, such as the adsorp-
dqt tion capacity and intensity. The Freundlich constants kf and n are
= k1 (qe − qt ) (7) determined from the intercept and slope, respectively, of the linear
dt
plot of log qe versus log Ce .
where qe (mg/g) and qt (mg/g) are the amounts of Mn adsorbed
on the adsorbent at equilibrium and at any time t (min), respec- Langmuir Isotherm
tively, and k1 (min−1 ) is the rate constant of the first-order model. The Langmuir isotherm model was developed to represent
The integrated form of the above equation with the boundary chemisorption at a set of well-defined localised adsorption sites
conditions t = 0 to >0 (q = 0 to >0) is rearranged to obtain the with the same adsorption energy, independent of the surface cov-
following time-dependence function: erage and with no interaction between adsorbed molecules. This
model assumes a monolayer deposition on a surface with a finite
k1 t number of identical sites. The Langmuir equation is valid for a
log(qe − qt ) = log(qe ) − (8)
2.303 homogeneous surface. The linearised form of Langmuir adsorp-
tion isotherm model is (Sohn and Kim, 2005; Demiral et al., 2008):
The first-order model considers the rate of occupation of the
adsorption sites proportional to the number of unoccupied sites. Ce 1 Ce
= + (13)
qe qm b Qm
Second-Order Lagergren Model
The Lagergren second-order kinetic model is expressed as where qe (mg/g) is the amount adsorbed at equilibrium, Ce
(Izanloo and Nassir, 2005): (mg/L) is the equilibrium concentration, qm is the Langmuir con-
stant representing maximum monolayer adsorption capacity and
dqt b is the Langmuir constant related to energy of adsorption.
= k2 (qe − qt )2 (9) The essential characteristics of the Langmuir isotherm can be
dt
expressed as the dimensionless constant RL (Oguz, 2004):
where k2 is the rate constant of second-order adsorption. The inte-
grated form of Equation (9) with the boundary condition t = 0 to RL =
1
(14)
>0 (q = 0 to >0) is: 1+bCo
| 450 | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | | VOLUME 91, MARCH 2013 |
and T is the temperature (K). The free energy change is obtained
using the following relationship:
G = −RT ln Kc (16)
G = H − T S (17)
S H
ln Kc = − (18)
R RT
Enhancement of adsorption capacity of electrocoagulant (mag- Figure 2. Effect of inter-electrode distance on removal efficiency and
nesium hydroxide) at higher temperatures may be attributed to energy consumption of manganese. Conditions—concentration: 2 mg/L;
the enlargement of pore size and or activation of the adsorbent pH of the electrolyte: 7.0; temperature: 305 K.
surface.
Pore Diffusion Coefficient (D) removal efficiency for the removal of Mn is 97.2% at pH 7 and the
The diffusion coefficient (D) for intraparticle transport of Mn minimum efficiency is 82.4% at pH 3. The decrease of removal
species into the adsorbent particles has been calculated at different efficiency at more acidic and alkaline pH was observed by many
temperature by: investigators and was attributed to an amphoteric behaviour of
Al(OH)3 which leads to soluble Al3+ cations (at acidic pH) and
r02 to monomeric anions Al(OH)4− (at alkaline pH). When the ini-
t1/2 = 0.03 × (19)
D tial pH was kept in neutral, all the aluminum produced at the
anode formed polymeric species (Al13 O4 (OH)7+24 ) and precipitated
where t½ is the time of half adsorption (s), ro is the radius of the Al(OH)3 leading to more removal efficiency. In the present study,
adsorbent particle (cm) and D is the diffusion coefficient (cm2 /s; the electrolyte pH was maintained in neutral, so the formation
Golder et al., 2006). of Mg(OH)2 is more predominant (like aluminium), leading to
greater removal efficiency.
RESULTS AND DISCUSSION
Effect of Inter-Electrode Distance Effect of Electrode Configurations
To determine the effect various inter-electrode distances between The percentage removal of Mn from Mg(OH)2 along with the
anode and cathode were kept at different spacing of 0.003, 0.005, experimental conditions utilised at various current densities from
0.007, 0.009 and 0.011 m using 2 mg/L Mn containing solutions 0.025 to 0.2 A/dm2 were analysed for monopolar and bipolar con-
at a current density of 0.05 A/dm2 . The results of inter-electrode figuration with concentration 2 mg/L. The data were presented in
distance on removal efficiency and energy consumption are pre- Table 1. From Table 1, it was observed that, for a given current
sented in Figure 2. While decreasing the inter-electrode distance densities, the removal efficiency of bipolar electrolytic cell was
shows decrease in energy consumption and increase in removal slightly higher than the monopolar electrode configurations. And
efficiency. Lower distance between anodes and cathodes require the energy consumption was higher for monopolar electrode than
low electrical energy for motion of ions. This is due to shorter the bipolar electrode.
travel path that reduce the resistance of motion of ions and the
situation is reverse for the case of large distance between each
electrode. In maintaining the inter-electrode distance of 0.003 m
was practically difficult. So, further experiments were carried out Table 1. Effect of electrode configuration at various current densities
at inter-electrode distance of 0.005 m. Inter-electrode spacing of with concentration 2 mg/L
0.005 m had the low energy consumption and removal efficiency.
Monopolar electrodes Bipolar electrodes
| VOLUME 91, MARCH 2013 | | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | 451 |
Figure 3. Effect of time on the amount of manganese-adsorbed qe at Figure 4. Second-order kinetic model plot of different current density of
various current density. Conditions—concentration: 2 mg/L; pH of the manganese. Conditions—concentration: 2 mg/L; temperature: 305 K; pH
electrolyte: 7.0; temperature: 305 K. of the electrolyte: 7.
Table 2. Comparison of experimental and calculated qe values at different current densities for first- and second-order adsorption kinetics of
manganese with concentration 2 mg/L at 305 K
Current density (A/dm2 ) qe (exp) qe (Cal) k1 × 104 (min/mg) R2 qe (cal) k2 × 104 (min/mg) R2
| 452 | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | | VOLUME 91, MARCH 2013 |
Table 2 depicts the computed results obtained from first- and
second-order models. From the results, it is observed that the
correlation coefficients for the first-order kinetic model were rel-
atively lower than those obtained for the second-order kinetic
model for the different current densities. These results indicate
that the second-order kinetic model can be applied suitably to
predict the Mn adsorption process onto magnesium hydroxides.
ISOTHERM MODELLING
Freundlich Isotherm
In testing the isotherm, the Mn concentration used was
0.5–2.5 mg/L with various current densities from 0.025 to
0.2 A/dm2 and at an initial pH 7. The adsorption data are plotted
as log qe versus log Ce by Equation (12) should result in a straight
line with slope n and intercept kf . The intercept and the slope
are indicators of adsorption capacity and adsorption intensity,
respectively. The value of n falling in the range of 1–10 indicates
favourable sorption. The kf and n values were listed in Table 3 for
Figure 5. Langmuir plot (1/qe vs. 1/Ce ) for adsorption of manganese.
each concentration and current density. It has been reported that Conditions—pH of the electrolyte: 7.0; current density:
values of n lying between 0 and 10 indicate favourable adsorption. 0.025–0.2 A/dm2 ; temperature: 303 K; concentration: 0.5–2.5 mg/L.
From the analysis of the results it is found that the Freundlich
plots fit satisfactorily with the experimental data obtained in the
present study. lated from Equation (14). The RL values were found to be between
0 and 1 for all the concentration of Mn studied.
Langmuir Isotherm
Langmuir isotherm was tested from Equation (13). The plots of
1/qe as a function of 1/Ce for the adsorption of Mn on Mg(OH)2 are
Thermodynamic Parameters
shown in Figure 5. The plots were found linear with good correla- Figure 6 shows that the rate constants vary with temperature
tion coefficients (>0.99) indicating the applicability of Langmuir according to Equation (15). The activation energy (0.665 kJ/mol)
model in the present study. The values of monolayer capacity (qm ) is calculated from the slope of the fitted equation. The free energy
and Langmuir constant (b) is given in Table 3. The values of qm change is obtained from Equation (16). The Kc and G values are
calculated by the Langmuir isotherm were all close to experimen- presented in Table 4. From the Table, it is found that the nega-
tal values at given experimental conditions. These facts suggest tive value of G indicates the spontaneous nature of adsorption.
that Mn is adsorbed in the form of monolayer coverage on the The enthalpy change (H = 3.063 kJ/mol) and entropy change
surface of the adsorbent. (S = 0.6975 J/mol K) were obtained from the slope and inter-
The applicability of the two isotherm equations was compared cept of the van’t Hoff linear plots of ln kc versus 1/T (Figure 7,
using the correlation coefficient (R2 ). The correlation coefficient Equation 17). Positive value of enthalpy change (H) indicates
values of Freundlich and Langmuir isotherm models are presented that the adsorption process is endothermic in nature, and the
in Table 3. The values of correlation coefficient (R2 ) are found to negative value of change in internal energy (G) show the spon-
be >0.9 for both isotherms. However, based on the R2 values, the taneous adsorption of Mn on the adsorbent. Positive values of
Langmuir isotherm model provided a better fit compared to Fre- entropy change show the increased randomness of the solution
undlich isotherm model. This suggests the adsorption of Mn by interface during the adsorption of Mn on the adsorbent (Table 4).
magnesium hydroxides is apparently with monolayer coverage of Enhancement of adsorption capacity of electrocoagulant (magne-
adsorbed molecules. The dimensionless constant RL were calcu- sium hydroxide) at higher temperatures may be attributed to the
enlargement of pore size and/or activation of the adsorbent sur-
face. Using Lagergren rate equation, second-order rate constants
and correlation coefficient were calculated for different tempera-
Table 3. Constant parameters and correlation coefficient for different tures (305–343 K). The calculated ‘‘qe ’’ values obtained from the
adsorption isotherm models for manganese adsorption at second-order kinetics agrees with the experimental ‘‘qe ’’ values
0.5–2.5 mg/L at various current densities of 0.025–0.2 A/dm2 better than the first-order kinetics model, indicating adsorption
following second-order kinetics. Table 5 depicts the computed
Current density (A/dm2 ) results obtained from first- and second-order kinetic models.
Freundlich kf (mg/g) 1.7125 1.5959 1.4321 1.3782 1.2566 Table 4. Thermodynamics parameters for adsorption of manganese
n (L/mg) 1.0026 1.0065 1.1061 1.0996 1.0664
R2 0.9885 0.9856 0.9823 0.9881 0.9876 Temperature (K) Kc G◦ (J/mol) H◦ (kJ/mol) S◦ (J/mol K)
Langmuir qm (mg/g) 1.7361 2.2261 2.8616 2.9465 3.0155
b (L/mg) 5.1892 4.9912 4.8321 4.5641 4.3981 323 17.085 −222.32 3.063 0.6975
R2 0.9995 0.9999 0.9989 0.9991 0.9988 333 18.122 −229.21
RL 0.5646 0.6125 0.5946 0.6864 0.6355 343 19.098 −236.17
| VOLUME 91, MARCH 2013 | | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | 453 |
Table 5. Comparison between the experimental and calculated qe values for the manganese concentration of 2 mg/L with 0.05 A/dm2 in first- and
second-order adsorption kinetics
Phosphate
The concentration of phosphate ion was increased from 0 to
50 mg/L, the contaminant range of phosphate in the ground water.
The removal efficiency for Mn was 97.2%, 96.3%, 64.7%, 41.5%
Figure 6. Plot of log k2 and 1/T. Conditions—pH of 7.0; current density:
0.025–0.2 A/dm2 ; concentration: 0.5–2.5 mg/L.
and 36.2% for 0, 2, 5, 25 and 50 mg/L of phosphate ion, respec-
tively. There is a negligible change in removal efficiency of Mn
below 2 mg/L of phosphate in the water was observed. At higher
concentrations (at and above 2 mg/L) of phosphate, the removal
Pore Diffusion Coefficient (D)
efficiency decreases drastically. This is due to the preferential
For all chemisorptions system the diffusivity coefficient should be adsorption of phosphate over Mn as the concentration of phos-
10−5 to 10−13 cm2 /s. In the present study, D is found to be in the phate increases.
range of 10−10 cm2 /s. The D values for various temperatures and
different initial concentrations of Mn are presented in Table 6.
Arsenic
The concentration of arsenic was gradually increased from 0 to
5 mg/L. From the results it is found that the removal efficiency
of Mn was decreased by increasing the concentration of arsenic.
The removal efficiencies are 97.2%, 95.7%, 83.5%, 73.6% and
54.6% for 0, 0.2, 0.5, 2.5 and 5.0 mg/L of arsenic, respectively.
Concentration (mg/L)
0.5 1.5229
1.0 1.1221
1.5 0.7847
2.0 0.5123
2.5 0.4838
Temperature (K)
323 2.5528
Figure 7. Plot of ln Kc and 1/T. Conditions: pH of the electrolyte: 7.0; 333 2.6318
current density of 0.025–0.2 A/dm2 ; concentration: 2 mg/L. 343 2.7109
| 454 | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | | VOLUME 91, MARCH 2013 |
This is due to the preferential adsorption of arsenic over Mn as
the concentration of arsenic increases. So, when arsenic ions are
present in the water to be treated arsenic ions compete greatly
with Mn ions for the binding sites.
Silicate
From the results it is found that no significant change in Mn
removal was observed, when the silicate concentration was
increased from 0 to 2 mg/L. The respective efficiencies for 0, 2, 5,
10 and 15 mg/L of silicate are 97.2%, 87.2%, 82.4%, 59.6% and
51.8%. In addition to preferential adsorption, silicate can interact
with magnesium hydroxide to form soluble and highly dispersed
colloids that are not removed by normal filtration.
SURFACE MORPHOLOGY
Characterisation of the Cathode Surface
To investigate the possibility of direct deposition of Mn on the
cathode surface, the EDAX analysis was carried out on the cathode
surface. The results showed that the amount of deposited Mn on
cathode surface is very low. The reason for this phenomenon may
be due to the hydrogen evolution from aqueous solutions will Figure 8. SEM image of the anode after treatment.
compete with metal deposition on the cathode surface. Hence, the
direct cathodic deposition has insignificant effect on the removal
of Mn ions from aqueous solution.
hydroxides. The formation of a large number of dents may be
Characterisation of the Anode Surface attributed to the anode material consumption at active sites due to
A SEM image of magnesium electrode after electrocoagulation of the generation of oxygen at its surface. The elemental constituent
Mn electrolyte was obtained (Figure 8). The electrode surface is of Mn-adsorbed magnesium hydroxide was shown in Figure 9. It
found to be rough, with a number of dents of ca. 10 um. These shows that the presence of Mn, Mg and O appears in the spectrum.
dents are formed around the nucleus of the active sites where EDAX analysis provides direct evidence that Mn is adsorbed on
the electrode dissolution results in the production of magnesium magnesium hydroxide.
| VOLUME 91, MARCH 2013 | | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | 455 |
The following conclusions were drawn based on the presented
information:
NOMENCLATURE
R2 regression correlation coefficient values
qt the amount of manganese adsorbate adsorbed on adsorbent
at any time (mg/g)
qe the amount of manganese adsorbate adsorbed on adsorbent
at equilibrium time (mg/g)
t time (min)
k1 the rate constant of first-order model (min)
k2 the rate constant of second-order model (L/g min)
Figure 11. XRD spectrum of manganese-adsorbed electrocoagulant. kf adsorption capacity of the Frendlich isotherm (mg/g)
n adsorption intensity of the Frendlich isotherm
Ce the non-retained manganese (mg/L)
MATERIAL CHARACTERISATION Co different concentrations of manganese (mg/L)
qm the maximum monolayer adsorption capacity (mg/g)
FT-IR and XRD Studies b energy of Langmuir adsorption
Figure 10 presents the FT-IR spectrum of Mn–magnesium hydrox- RL Langmuir equilibrium constant
ide. The sharp and strong peak at 3694.57 cm−1 is due to the (O–H) ko thermodynamical Arrhenius constant (g/mg min)
stretching vibration in the Mg(OH)2 structures. The 1476.6 cm−1 E energy of activation (J/mol)
peak indicates the bent vibration of H–O–H. A broad absorption R gas constant which is 8.314 (J/mol K)
band at 3696.4 cm−1 implies the transformation from free pro- T Temperature (K)
tons into a proton conductive state in brucite. The strong peak at G Gibbs free energy for adsorption (kJ/mol)
439.2 cm−1 is assigned to the Mg–O stretching vibration (Golder et Kc equilibrium constant of adsorption process
al., 2006; Vasudevan et al., 2010). The spectrum data are in good H enthalpy of the adsorption (J/mol)
agreement with the reported data (Golder et al., 2006). Mg–Mn S entropy of the adsorption (J/mol)
is observed in –OH stretching region. The Figure 11 shows the X- t½ half time of adsorption (min)
ray diffraction of Mn-adsorbed magnesium hydroxide. From the D diffusion coeffficient (cm2 /s)
figure it is found that electrocoagulation by product showed the r0 radius of the particle (cm)
well crystalline phase of magnesium hydroxide.
ACKNOWLEDGEMENTS
CONCLUSIONS The authors wish to express their gratitude to the Director, Cen-
The results indicate that the electrocoagulation is a promis- tral Electrochemical Research Institute, Karaikudi to publish this
ing technology for the removal of Mn from drinking water. article.
| 456 | THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING | | VOLUME 91, MARCH 2013 |
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