Case Studies in Chemical and Environmental Engineering 2 (2020) 100061

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Case Studies in Chemical and Environmental Engineering

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Corrugated iron sheets for electrocoagulation of sulphate ions in

industrial effluents
Siyanda Yamba a, c, Richard Motlhaletsi Moutloali a, b, Nonhlangabezo Mabuba a, *
a
Department of Chemical Sciences, University of Johannesburg, P.O. BOX 170111, Doornfontein, 2028, South Africa
b
Department of Science and Technology/Mintek- Nanotechnology Innovation Centre, University of Johannesburg, Johannesburg, South Africa
c
Buffalo City Metro Municipality, Scientific Services, No.1 Reservoir Road, Selbone, East London, 5201, South Africa

A R T I C L E I N F O A B S T R A C T

Keywords: High sulphate concentrations in industrial effluents damage municipality infrastructures. Old corrugated iron was
Industrial effluents used as an electrode to remove SO2-4 concentration in industrial effluents. Electrodes were characterized using SEM
Water treatment and EDS. The optimised parameters were pH 2, 3000 ppm, 15 V and 120 min. In an industrial effluent, 99% of
Electrode platform
SO2- 2- -
4 was removed including PO4 , F and COD. The sulphates were physically adsorbed on Zn and Fe hydroxides
Sulphate concentration
Municipality water
according to first order kinetics. The corrugated iron is reusable and consumed low energy (0.1725 kWh/m3).

1. Introduction co-authors [14]. A current density of 25 mA/cm2 was effective to

South African municipal wastewater treatment plants are destroyed
by industrial effluents that contain high sulphate concentration. These
effluents emerge from textile, battery, pulp and paper, acid mine water as
well as food manufacturing industries [1]. According to the municipal
by-laws, permissible sulphate (SO2
4 ) concentration range should be be-
tween 200 and 400 ppm [2]. High sulphate concentration in industrial
effluents corrodes pipes, cracks cement walls, destroys the infrastructure
and hinders service delivery to the communities. The aforementioned has
a negative impact in the economy as a lot of finances are spent on repairs
caused by excess sulphates in water.
Consequently, sulphate monitoring is becoming stringent and various
regulations have been set for its concentration in water [3–6]. Hence,
technologies that have been developed to mitigate SO2
4 ions in water
include chemical precipitation, ion exchange resins and membrane pro-
cesses to name a few [6–8]. Membrane processes are reported as energy
intensive and prone to fouling, while chemical precipitation methods
result in secondary pollution due to toxic sludge formation [9,10].
Alternatively, electrocoagulation technique has been projected as a
promising technique to treat various wastewaters, such as landfill
leachate, restaurant wastewater, saline wastewater, tar sand and shale
wastewater, urban wastewater, laundry wastewater, nitrate and arsenic
bearing wastewater and chemical-mechanical polishing wastewater
[11–13]. The electrocoagulation of sulphate using aluminium anodes in
bipolar and monopolar configurations was reported by Nariyan and
decrease sulphate from 1300 ppm to 250 ppm, which is the acceptable


limits in most mining companies. In addition, Del Angel et al. carried out
electrocoagulation experiments by employing aluminium electrodes, and
obtained 53% of sulphate removal from the abandoned mine drainage
with an initial concentration of 3567 mg/L [15]. Radi
c et al. reported
more than 86% removal percentage of sulphate from acid mine drainage
(initial concentration was 10,830 mg/L) with combined CaO/elec-
trocoagulation treatment [16].
The results of Garcia-Sugura and co-authors indicated that in situ
electrocoagulation is more efficient because it mitigates the pollutants in
real environment compared to the lab based methods [17]. In general,
the principle of electrocoagulation method depends strongly on sacrifi-
cial anode, cathode, metal solubility and pH of water [18–20]. The anode
is oxidized to metal cation which is used as an in situ developed coagu-
lant for anions while water is reduced to hydrogen gas and hydroxyl
anions at the cathode (Equations (1) and (2)). Consequently, the metal
cations and hydroxyl anions form metal hydroxide precipitate (Equation
(3)). The soluble contaminants can be removed from water by chemical
or physical adsorption onto the metal hydroxides. As the oxygen evolu-
tion occurs, Fe2þ is oxidized to Fe3þ which also forms iron hydroxide
flocs to remove pollutant ions (Equation (4)). Alternatively, the pollutant
act as a ligand (L) to form an insoluble complex with the metal hydroxide
(Equation (5)) [17].
Fe (s) → Fe2þ (aq) þ2e
Eq.1

* Corresponding author.
E-mail address: nmabuba@uj.ac.za (N. Mabuba).

https://doi.org/10.1016/j.cscee.2020.100061
Received 17 March 2020; Received in revised form 20 November 2020; Accepted 23 November 2020
2666-0164/© 2020 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
S. Yamba et al.
2H2O (l) þ 2e
→ H2 (g) þ 2OH
(aq) Eq.2
Fe2þ (aq) þ 2OH
(aq) → (OH)2 (s) Eq.3
2þ þ
4Fe (aq) þ 10H2O (l) þ O2 (g) → 4(OH)3 (s) þ 8H (aq) Eq.4
L-H (aq) þ (OH)OFe (s) → L-OFe (s) þ 2H2O (l) Eq.5
The advantage of electrocoagulation is that the water treatment is
performed without adding any chemical coagulants or flocculants which
may otherwise lead to secondary pollution. Hence, this work explores the
use of recycled, inexpensive corrugated iron electrode as a sacrificial
electrode to determine its efficiency in the removal of sulphate ion to
permissible limit.
2. Materials and methods
2.1. Preparation of solutions
The study employed Sodium sulphate (97% purity), Hydrochloric
acid (37%), and Sodium hydroxide pellets (97% purity) were purchased
from Merck. All the glassware was soaked in 5% HNO3 for 24 h followed
by washing them three times with Millipore water and air drying. Syn-
thetic sulphate solutions were prepared from Na2SO4 using deionised
water. The effect of initial sulphate ion concentration was studied by
varying its concentration from 2000, 3000, 4000, 5000 and 6000 ppm,
while other parameters such as, pH, contact time, and voltage were kept
constant.
The initial pH of the solutions was measured using a HACH HQ 440d
multimeter (Germany) was adjusted to pH ranging from 2 to 10 using 0.5
M HCl and 0.5 M NaOH which were purchased from Sigma Aldrich
(South Africa). Ultrapure water (18.2 MOhm cm at 22  C) was used to
make all solutions used.
2.2. Experiment configuration
An electrocoagulation unit was constructed using a TINTEK-PW 3033
power supply. The corrugated iron sheets (area of 21cm2) were collected
from a local metal scrap yard. They were immersed in a beaker con-
taining sulphate solution, and a stirrer plate was used to maintain ho-
mogeneity. The corrugated iron sheets were set up in monopolar
alignment by connecting an anode and a cathode with 1 cm distance
between electrodes for all experiments. For all experiments, an effective
area of 21 cm2 for each electrode was immersed into water in the beaker.
The voltage (3–15 V) was applied from 20 to 120 min, during which the
water was stirred with a magnetic stirrer at 200 rpm.
The pH of the working solution was adjusted by adding dilute hy-
drochloric acid or sodium hydroxide. After each experiment, the elec-
trodes were softly rubbed with sand paper to remove scaling and refine
the surface, followed by washing with ultrapure water. Subsequently,
electrocoagulation proceeded for 120 minutes and the solution was left
to cool down. The precipitate was filtered off and the filtrate was ana-
lysed for sulphate concentration.
The electrodes were characterized by scanning electron microscopy
(SEM) and energy dispersive spectroscopy (EDS) to evaluate changes in
morphology and elemental composition of the corrugated iron (electrode
where electrocatalysis takes place) before and after electrocoagulation.
2.3. Sampling and analyte detection method
Different industrial effluents from Buffalo City Metro, South Africa
were collected and analysed. The effluents were analysed for various
parameters such as pH, chemical oxygen demand, sulphate (SO2
4 ),


phosphate (PO2
4 ), and fluoride (F ) to determine the electrocoagulation
performances.
2
Case Studies in Chemical and Environmental Engineering 2 (2020) 100061
The extent of sulphate removal was determined according to the
standard detection of water and wastewater [21]. The sulphate synthetic
samples and industrial effluents were analysed using a spectrophotom-
eter (HACH DR900, Germany). The limit of quantification (LOQ) and
limit of detection (LOD) were quantified using Equations (6) and (7),
respectively Where, SB is the relative standard deviation of the blank,
and m is the slope obtained from the calibration data.
10  SB
LOQ ¼ Eq. 6
m
3  SB
LOD ¼ Eq. 7
m
The removal percentage was calculated using the following equation
(8):
CO
C
%Removal ¼ x 100 Eq. 8
CO
where C0 and C are the initial and final sulphate concentrations (mg/L),
respectively.
An OPTMA PerkinElmer 5300 DV ICP-OES (USA) was used to monitor
zinc dissolution during the electrocoagulation process. All analysis or
tests were repeated in triplicate to ensure reproducibility of the data, and
all the data in the figures and tables were averaged.
2.4. Kinetics study
In order to study whether the sulphate was chemically or physically
adsorbed onto the iron hydroxide precipitate the pseudo first-order
(Equation (9)) and pseudo second-order for chemical adsorption (Equa-
tion (10)) kinetics models were fitted into the experimental results at
different voltage application (6 V, 9 V and 15 V), respectively [22].
ln Ct ¼ ln C0
k1 t Eq. 9

1
Ct ¼ k2 t þ 1= Eq. 10
C0
where C0 (mg/L) is the initial sulphate concentration and Ct is the sul-
phate concentration at time t; k1 (min
1) and k2 ((mg/L)
1 min
1) are the
pseudo first-order and pseudo second- order constants, respectively.
2.5. Energy consumption of electrocoagulation process
In electrocoagulation process, electrical energy consumption (EEC) is
the major factor that affect operating cost (kWh/m3). In order to reduce
economic and environmental impacts, less energy consumption is
required. Equation (11) was applied to calculate the energy used during
electrocoagulation [23].
UxIxt
ECC ¼ Eq. 11
60xV
where, EEC is the electrical energy consumption (kWh/m3), U is the
applied voltage (V), I is the current (A), t for the reaction time (min) and
V is the volume (dm3) of the treated water.
2.6. Reusability of the corrugated iron (electrode)
A single electrode (at 15 V) was used five times (cycles), to treat water
samples containing 2663 ppm SO2
4 and other ions, at pH ¼ 4.41. The
electrodes were in contact with the SO2
4 solution for 120 min in each
cycle, then washed and dried for the next cycle.
S. Yamba et al. Case Studies in Chemical and Environmental Engineering 2 (2020) 100061

3. Results and discussion Table 1

Elemental composition of anode before and after the electrocoagulation process.
3.1. Characterization of corrugated iron electrode Elements Electrode composition Elements Electrode composition after
before electrocoagulation electrocoagulation
To gain the insight on the morphological and composition changes Weight (%) Atomic (%) Weight (%) Atomic (%)
that occur on the surface of electrodes before and after electro-
C 18.22 37.92 C 18.67 46.76
coagulation, SEM coupled with EDS was used. The surface characteristics O 25.05 39.13 O 6.27 11.78
have an effect in the effectiveness and lifespan of the electrodes used. Al 0.95 0.88 Al 1.75 1.95
Fig. 1a displays a rough micro-surface, with irregular voids and marks Si 0.89 0.79 Si 0.18 0.19
due to corrosion or rusting of corrugated iron when exposed to outdoor S 0.29 0.23 Fe 72.08 38.83
Cl 0.37 0.26 Zn 1.06 0.49
environment. After electrocoagulation as displayed in Fig. 1b a smooth,
K 0.15 0.10 – –
straight-lined microstructure of the corrugated iron electrode was ob- Cr 0.23 0.11 – –
tained, suggesting that the coating on top layers of the electrodes dis- Zn 53.85 20.59 – –
solved uniformly during electrolysis.
Table 1 indicates the elemental composition of the corrugated iron
electrodes/sheets before and after electrocoagulation. This investigation At the cathode, the water is reduced to hydroxide and hydrogen. The
confirmed that before the electrocoagulation process, the old corrugated hydroxide forms a zinc hydroxide and iron hydroxide which also
iron sheet contained high zinc and oxygen content (due to rust). Nor- precipitated (formed flocs) due to the hydrogen from the cathode at pH 3
mally, the zinc layer is present as corrosion protection for iron, which is as summarised chemical equations (13) and (15) [24]. Thereafter, the
usually done by galvanization. When the scrap metals are used as sacri- zinc (II) and iron (II) hydroxides participated in sulphate adsorption at
ficial electrodes, the Zn coating is oxidized and also act as coagulant for pH 3 [17,18,20,24,25].
sulphates, fluorides and phosphates in water [24]. In alkaline media, the evolution of oxygen enhanced the oxidation of
some of Fe2þ to Fe3þ which formed iron (III) hydroxide as displayed in
equation (16). As the pH increased from 6 to 10, the removal percentage
3.2. Optimization studies and sulphate removal mechanism decreased due to low concentration of soluble Fe2þ and cation hydrox-
ides can be negatively charged hence 20% sulphate was removed [18,
In acidic media with a low pH (2), higher percentages of sulphates 25].
(95.4%) were removed (Fig. 2a). The mechanisms of sulphate removal
Zn (s) → Zn2þ (aq) þ2e
Eq. 12
depend on the solubility of the sacrificial electrode elements into the
2þ

sulphate solution [19,24]. According to Faraday’s theory the mass of the Zn (aq) þ 2OH (aq) þSO24 (aq) →Zn(OH)2 (s) þ SO2

4 (aq) Eq. 13
solute in solution was 3.025 g which confirmed that there were several
reactions that contributed towards the mechanisms of sulphate removal Fe (s) → Fe2þ (aq) þ 2e
Eq. 14
[18,25]. The reactions for sulphate removal included the oxidation of Fe2þ

(aq) þ OH (aq) þ SO2
SO2

4 (aq) → Fe(OH)2 (s) þ 4 (aq) Eq. 15
zinc and iron at the anode according to Equations (12) and (14) [24].
2þ
Thereafter, the cations (Zn2þ and Fe2þ) are electrostatically attracted to 4Fe (aq) þ10H2O (l) þ O2 (g) → 4(OH)3 (s) þ8Hþ (aq) Eq.16
sulphates in solution into forming chemical precipitate at pH 2 [25].
It is evedent from Fig. 2b that increasing initial sulphate concentra-
Thus, chemisorption of negatively sulphate on the positively charged
tion, decreased the removal percentage from 95% at 2000 ppm to 40% at
surface of the coagulants is favoured. The Fe2þ and Zn2þ (coagulants)
high sulphate concentration such as, 6000 ppm. Fig. 2c indicates results
concentrations persisted longer thus higher concentrations of sulphates
for varying voltage against sulphate removal percentage. This study
were removed.

Fig. 1. SEM image of an old corrugated iron sheet (A) before and (B) after electrocoagulation.

3
S. Yamba et al. Case Studies in Chemical and Environmental Engineering 2 (2020) 100061

Fig. 2. Optimization of parameters, effect of (a) pH, (b) initial SO2

4 concentration, (c) voltage applied and (d) contact time.

suggested that there was a drastic increase in sulphate removal per-

Table 2
centage (from 59.5 to 95.4%) with increased voltage. This was attributed
Components of Wastewater treatment before and after the electrocoagulation
to the fact that at higher voltage, more iron concentrations were oxidized
process.
into the water. Thus, iron hydroxide precipitate (flocs) were formed and
Parameters Industrial Removal Synthetic Removal Discharge
they adsorbed more sulphate ions from solution. It was easy to filter the
effluent (%) effluent (%) Limitsa
flocs off from the solution. (mg/L) (mg/L) (mg/L)
The effect of contact time on the removal percentage of sulphate by
SO2

4 2678 99 3000 95 500
eletrocoagulation process is shown in Fig. 2d, which indicated that more
PO3

4 106 94 150 91 25
than 75% sulphate removal was obtained in 60 min treatment time, using F

60 94 100 90 5
the corrugated iron electrodes. As time elapsed, 95% of sulphate con- COD 1459 90 1000 89 700
centration was removed in 120 min. pH 4.39 – 2 – 6–11
The following parameters, pH, initial concentration, voltage and c
BCMM By-Laws (No 2532).
contact time were optimised to 2, 3000 ppm, 15 V, 120 min, respectively.
These optimised parameters were applied in industrial and synthetic concentration was removed. In the synthetic sample, PO3


4 , F and COD
sample analysis in section 3.3. removal percentages were above 70%. These attributes of the electro-
coagulation present a fundamental scope in its application to wastewater
3.3. Sulphate removal from industrial effluents and synthetic solutions treatment which enables effluents to be discharged into the sewer
framework without pH adjustment (as pH is always balanced to
The slope of the calibration curve was used to determine the sensi- neutrality at the end of electrocoagulation).
tivity of the method, and was found here to be 0.0779 and correlation
coefficient (R2) was found to be 0.9905. The linearity was acceptable and 3.4. Energy consumption of electrocoagulation process
applied to obtain accurate sulphate concentration from unknown sample.
The limit of detection (LOD) and limit of quantification (LOQ) were At optimised conditions, the results (Fig. 3) demonstrated that by
0.114 ppm and 0.36 ppm. Each analysis was repeated three times and the increasing contact time from 20 to 120 min, electrical energy con-
relative standard deviation was 1.62. sumption linearly increased from 0.02588 to 0.1725 kWh/m3 at 15 V,
An industrial sample containing high sulphate concentration (~2678 which lies within the acceptable electrocoagulation range 0.002–58
ppm) above permissible limits, was used as a real sample (Table 2) under kWh/m3 [24]. The optimised voltage was 15 V, due to high sulphate
optimised experimental parameters. After electrocoagulation with removal percentage at low electrical energy consumption (0.1725
corrugated iron electrodes, a decrease in sulphate content to 37 ppm was kWh/m3).
observed, equivalent to a 99% SO2
4 concentration removal. This value
falls within the permissible limits, as specified by the Buffalo City Metro 3.5. Reusability of the corrugated iron (electrode)
Municipality (BCMM) by laws. Other ions within the industrial effluent


such as PO3
4 and F were also removed during the electrocoagulation The efficiency and reusability of the corrugated iron electrodes were
process (~94% removal). Also, chemical oxygen demand (COD), which evaluated by the reuse of a single electrode for 5 cycles, in real industrial
is another problem during treatment of industrial wastewaters [26], is water sample containing 2663 ppm SO2
4 concentration and other ions.
reduced within permissible limits after electrocoagulation. A similar The optimised voltage (15 V) and time (120 min) were applied. Fig. 4a
trend was observed in synthetic samples, where 80% of the sulphate displayed that corrugated iron electrodes can be used up to 3 times to

4
S. Yamba et al. Case Studies in Chemical and Environmental Engineering 2 (2020) 100061

and Fe2þ in solution. Low Zn2þ and Fe2þ concentrations were confirmed
by the decrease in the mass of an electrode from 3.21 g to 2.79 g (Fig. 4b)
as the number of cycles were increased. Therefore, the corrugated elec-
trode may be applied for 3 cycles with an energy consumption of 0.1725
kWh/m3 to remove sulphate concentration.

3.6. Kinetics study

Results in Fig. 5a and b indicated that the data for the removal of
sulphate concentration obeyed the first order kinetics with good corre-
lation coefficients (R2) of 0.9983, 0.9982 and 0.9984 at different voltages
(6, 9 and 15V). The R2 in second order were 0.8921, 0.89620 and 0.8942,
which were lower than the first order. The information confirmed a
physical adsorption of sulphates to the zinc(II) and iron (II) hydroxide
precipitates. Furthermore, the rate constants increased with increasing
voltage applied. The values of rate constants at optimum conditions are
presented in Table 3.

4. Conclusion
Fig. 3. Effect of applied voltage on energy consumption at opti-
mised conditions.
The study presented the use of an inexpensive, recycled corrugated
iron as a sacrificial electrode (anode) in removal of 99% sulphate con-
decrease the concentration of sulphate ions in the real water sample

centration and other water parameters (PO3
4 , F and COD) from in-
(initially 2663 mg/L) to 37 ppm, equivalent to 99% SO2
4 removal. dustrial effluents. The high percentages of sulphate concentration were
Increasing the number of cycles or reuse further than this, resulted in removed by adsorption of sulphate ions onto the zinc(II) and iron (II)
decreased removal percentage of 40% due to lower concentration of Zn2þ hydroxides precipitate (flocs) in solution. The corrugated iron electrodes

Fig. 4. a) Reusability of a corrugated iron electrode b) Mass loss in corrugated iron electrode under optimised conditions.

5
S. Yamba et al. Case Studies in Chemical and Environmental Engineering 2 (2020) 100061

Fig. 5. a) fist order and b) second order kinetic studies for sulphate removal at optimal parameters.

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