Accepted Manuscript

Investigation of electrocoagulation reactor design parameters effect on the re-

moval of cadmium from synthetic and phosphate industrial wastewater

Brahmi Khaled, Bouguerra Wided, Hamrouni Béchir, Aloui Limam, Loungou

Mouna, Zied Tlili

PII: S1878-5352(14)00362-1
DOI: http://dx.doi.org/10.1016/j.arabjc.2014.12.012
Reference: ARABJC 1523

To appear in: Arabian Journal of Chemistry

Received Date: 2 October 2014

Accepted Date: 27 December 2014

Please cite this article as: B. Khaled, B. Wided, H. Béchir, A. Limam, L. Mouna, Z. Tlili, Investigation of
electrocoagulation reactor design parameters effect on the removal of cadmium from synthetic and phosphate
industrial wastewater, Arabian Journal of Chemistry (2015), doi: http://dx.doi.org/10.1016/j.arabjc.2014.12.012

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 Investigation of electrocoagulation reactor design parameters effect on the removal of
cadmium from synthetic and phosphate industrial wastewater

BRAHMI Khaled a, BOUGUERRA Wided a, HAMROUNI Béchir a, ALOUI Limam b, LOUNGOU Mouna c, Zied Tlili d
a U. R Traitement et Dessalement des Eaux, Département de Chimie,
Faculté des Sciences de Tunis, 2092 Manar II, TUNISIE, Tel./ Fax: +2167187128.
b U. R Matériaux, Environnement et Energie, Département de Chimie,
Faculté des Sciences de Gafsa, Campus Universitaire Sidi Ahmed Zarroug -2112 Gafsa, TUNISIE, Tel +216 76 211 026.
c Groupe Chimique Tunisien, Usine de M’Dhilla Gafsa, Km. 14 Route M’Dhilla- 2100 Gafsa, Tel +216 76211515.
d Higher Institute of Business Administration of Gafsa, Campus Universitaire Sidi Ahmed Zarroug -2112 Gafsa, TUNISIE, Tel +216 24951825.
Tel./ Fax: +21671871282; Corresponding author E-mail:khaled.brahmii@gmail.com

ABSTRACT

This study investigates the effect of reactor design parameters on cadmium removal from
industrial wastewater discharged by the Tunisian Chemical Group (TCG) to improve as much
as possible efficiency and cost of electrocoagulation (EC) process. Based on an examination of
the design parameters one by one, the best cadmium removal was achieved for an
inter-electrode distance (die) of 0.5 cm, monopolar connection mode, stirring speed of 300 rev
min-1, surface-area-to-volume ratio (S/V) of 13.6 m-1, and an initial temperature of 50 C°. These
operating conditions allowed to achieve efficient removal in a relatively short operating time
with the lowest energy consumption and cost possible. The present study proved that the
parameters that have an effect on the operating cost are the electrode configuration,
inter-electrode distance and S/V ratio. The energy consumption, the pH evolution, and the
treatment cost were studied. The investigation of the effect of all the selected optimum EC
design parameters together on the removal of cadmium from the TCG wastewater proved that
the treatment was highly efficient; 100 % of cadmium removal was reached in 5 min, with a
very low power consumption (1.6 kWh m-3) and very low cost (0.116 TND m-3). Moreover, EC
was found to be capable of removing cadmium as well as other pollutants at the same time from
the case-study industrial wastewater. The investigation carried out in this work explores and
proposes a very cost-effective treatment method to remove heavy metals from industrial
wastewater if compared to results reported about cost of this treatment process through other
widely used technologies such as coagulation (4.36 Tunisian National Dinar (TND) m-3) and
precipitation (9,96 TND m-3) employed in previous studies.

Keywords: Wastewater treatment; Electrocoagulation; treatment cost; Investigation of reactor

design parameters; Cadmium removal; Energy consumption.

1
1. Introduction

The removal of heavy metals from industrial waste has become one of the most essential
applications in wastewater treatment in terms of protection of health as well as the environment.
These heavy metals are known to be among the most common pollutants found in industrial
wastewaters and pose serious health hazard, and are environmentally-unfriendly because they
are not biodegradable and tend to accumulate in living organisms (Saha and Sanyal, 2010).
Cadmium is a toxic non-essential heavy metal in the environment; it is teratogenic and
carcinogenic (Young, 2005). Cadmium toxicity causes renal damage (Suwazono et al. , 2000),
pulmonary insufficiency and negative effects on bones, liver and blood (IRAC, 2006).
Cadmium poisoning, therefore, creates far greater likelihood of weaker and weaker constitution
of such parts of the body obviously performing vital bodily functions. The drinking water
guideline value is 0.005 mg L-1 (Health Canada, 2012).
The increased water use and wastewater discharge, particularly industrial wastewater,
have added impurities to water which requires cleaning processes (Vasudevan and Lakshmi,
2011). It is important to note that the overall treatment cost of metal-contaminated water varies,
depending on the process employed and the local conditions. In general, the technical
applicability, simplicity and cost-effectiveness are the key factors in selecting the most suitable
treatment of inorganic effluent. Physical methods like ion exchange, reverse osmosis and
electrodialysis have proven to be either too expensive or inefficient to remove cadmium from
water (Vasudevan and Lakshmi, 2011). During the past few years, EC has been proposed as an
effective method to treat many types of effluents such as wastewater charged with heavy metals
(Kumar et al. , 2004), natural water charged with Fluor (Emamjomeh and Sivakumar, 2006),
surface water (Lai and Lin, 2006), suspended solids, oil and fat in restaurant wastewater (Chen
et al. , 2000), black liquor from paper industry (Zaieda and Bellakhala, 2009), and cigarette
factory wastewater (Bejankiwar, 2002). All these investigations showed that EC could achieve
a significant reduction of major pollutants and has become of growing interest for the industrial
scale.
EC is a simple and efficient process where the production of the coagulating agent is
managed in situ by means of electro-oxidation of a sacrificial anode. In this case, there is no
need for adding chemical coagulants or flocculants to perform the treatment (Elham et al. ,
2011). In the EC process, the destabilization mechanism of the contaminants, particles
suspension, and breaking of emulsions can be summarized as three successive steps: (1)
compression of the diffuse double layer around the charged species by the interactions of ions
2
generated by oxidation of the sacrificial anode, (2) charge neutralization of the ionic species
present in wastewater by counter ions produced by the electrochemical dissolution of the
sacrificial anode. These counter ions reduce the electrostatic inter-particle repulsion to the
extent that the van der Waals attraction predominates, thus causing coagulation. A zero net
charge results in the process, and (3) flocs formation; the flocs formed as a result of coagulation
creates a sludge blanket that entraps and bridges colloidal particles that are still remaining in the
aqueous medium (Thirugnanasambandham et al. , 2013). The EC has been used for treatment of
various types of wastewater and effluents containing algae, phosphate, sulfide, sulfate, sulfite,
fluoride and heavy metals ions such as; Fe2+, Ni2+, Cu2+, Zn2+, Pb2+, Cd2+ (Emamjomeh and
Sivakumar, 2009; Merzouket al. , 2009; Lekhlif et al. , 2014; Rajesh et al. , 2014; Umran et al. ,
2015). The proposed mechanism of chemical reactions occurring in the EC process is shown by
the following main reactions at the aluminum electrodes (Ilhan et al. , 2007) :

Anode: Al(s) ↔ Al3+ (aq) + 3 e- Eq. (1)

Cathode: 3 H2O (aq) + 3 e- ↔ 3/2 H2 (g) + 3 OH - (aq) Eq. (2)

The hydroxyl ions produced at the cathode increase the pH in the electrolyte and we
have a reaction in the aqueous solution between Al3+ and OH- ions to form aluminum
hydroxide:

In bulk: Al3+ (aq) + 3OH- (aq) ↔ Al (OH)3 (s) Eq. (3)

In the presence of sufficiently high potential, secondary reactions such as direct

oxidation of organic compounds and of H2O or Cl- are also likely to occur at the anode present
in wastewater. These reactions are shown by the following main reaction:

In bulk: 2 Cl - (aq) ↔ Cl2 (g) + 2 e- Eq. (4)

In bulk: 2 H2O (aq) ↔ O2 (g) + 4 H+ (g) + 4e- Eq. (5)

The chlorine produced is a strong oxidant that can oxidize the same organic compounds
and promote electrode reactions. The generated Al3+ ions would immediately undergo further
spontaneous reactions to produce corresponding hydroxides and/or poly-hydroxides in a wide
pH range. These hydroxides/ poly-hydroxides/poly-hydroxy metallic compounds such as
Al6(OH)153+, Al7(OH)174+, Al8(OH)204+, Al13O4(OH)247+, Al13(OH)345+, which transform finally

3
into Al(OH)3 according to complex precipitation kinetics, have a strong affinity with
dispersed/dissolved ions as well as the counter ions to cause coagulation/adsorption. The
advantages of EC include high removal efficiency, a compact treatment facility, relatively low
cost, and the possibility of complete automation (Vasudevan and Lakshmi, 2011).
The effect of EC reactor design parameters on the treatment of wastewater has received
a great deal of attention in the existing literature on the utilization of EC technology (Chopra et
al. , 2011; Rajesh et al. , 2014; Umran et al. , 2015), yet it seems that previous studies have not
set out to apply all design parameters at the same time to achieve high rate of removal efficiency
much more cost-effectively. The present study was designed to investigate the effect of reactor
design parameters on cadmium removal from industrial wastewater one by one then apply their
optimal yields on the treatment of the case-study wastewater in order to improve as much as
possible the efficiency of EC process and significantly reduce its cost as well. Different
parameters such as the surface-area-to-volume ratio, the inter-electrode distance, the state of the
aluminum plates, the stirring speed, the electrodes configuration mode and the initial
temperature of water were studied in detail. EC-based process was applied on the treatments of
wastewater discharged from phosphate and acid manufacturing TCG in M’Dhilla, Gafsa,
Tunisia, which is highly acid (pH = 2.02) and contains large amounts of heavy metals. This
industry consumes 400 m3 day-1, yet the treatment of this particular hazardous wastewater
containing large quantity of cadmium has never been studied in previous research. This
investigation sets out to achieve high-rate cadmium removal from TCG industrial wastewater
cost-effectively. Additionally, the treatment process carried out in this study enables the
reusability of the case-study wastewater and thus could allow a significant reduction in water
consumption, and promises to be very useful for further applications of the EC process on the
treatment of wastewater containing heavy metal ions.

2. Materials and methods

2.1. Reagents and analytical procedures

All the chemicals used were of analytical grade. Total Cadmium concentration was
determined by using flame atomic absorption spectroscopy (FAAS) method. The conductivity
was measured during the experiments using the conductivity meter Jenway 4510 (Ω Metrohm).
A calibrated Digital pH-meter Cyber Scan 510 (WDW, Germany) was used to measure the pH
and the temperature of the solution.

4
2.2. Validation of the analytical method

The flame atomic absorption spectroscopy (FAAS) method was used to determine
cadmium concentration. This method was the most feasible one because it could be adequately
adapted to higher concentration of the cadmium measurement. The flame atomic absorption
spectroscopy Analytik Jenna Nova 400 was used. In order to perform the experiments and
assure the reliability and validity of the atomic absorption method whereby residual cadmium
(II) concentration could be determined, several tests had been done to calculate the linearity,
specificity, fidelity (reproducibility and repeatability) as well as limits of both instrumental
method detection and quantification. The result of the experimental validation of the atomic
absorption analytical method is shown in table.1. The method for Cd(II) determination by
AASF is efficient, with a detection limit of 0.0187 and a quantification limit of 0.0624 in a
range of linearity of 0.02 to 2 mg L-1.

2.3. Cell construction

The experimental setup is shown in Fig. 1. The EC cell was made up of 1L cylindrical
Plexiglas beaker, with a wooden cover supporting the set of parallel aluminum sheets used as
sacrificial electrodes. The electrodes used in this work were formed by two parallel rectangular
aluminum plates (250 mm * 80 mm * 2 mm). The total immersed area of each electrode was
active (85mm * 80mm * 2mm) S = 68 cm2, the other section of the electrodes was wrapped and
inactivated with a durable water-resistant sellotape in order to fix the immersed area and avoid
the anode loss. The anode-cathode spacing was varied from 5 to 20 mm. A small hole was
drilled in the cover to serve as a sampling port. The experimental runs were performed at a
magnetic stirring speed varied from 0 to 600 rev min-1.

2.4. Treatment procedure

The treatments were carried out using aluminum as electrodes. Before each treatment,
and in order to avoid a passivation film, the electrodes (anode and cathode) were rubbed with
sandpaper then cleaned with NaOH (2 M) and HCl (2 M) aqueous solutions. The solutions were
prepared using CdSO4, 10 H2O. If required, the pH of the electrolyte was adjusted with HCl (0.
1 M) and NaOH (0. 1 M) solutions before each EC test started. The current intensity was
maintained at the range from 0 to 3 A using a regulated direct current power supply (DC) AFX
2930 SB DC and the voltage cell between the electrodes was continuously recorded. As has
been already noted, the wastewater under investigation was collected from a Tunisian sulfuric

5
acid and superphosphate manufacturing industry. Sample filtration, collection and preservation
were carried out immediately in the industry laboratory of quality control of TCG. For each
sample, cadmium concentration was measured three times to determine the average
concentration as a result with respect to reproducibility and repeatability. The investigation of
the EC reactor design parameter using aluminum electrodes was carried out for an initial
concentration of 100 ppm keeping constant the volume of the solution (1L), the current density
(j) at 3.68 mA cm ², the initial pH at 7, the conductivity ( ) at 5.86 mS cm-1. Only the studied
parameter was varied, in order to clearly show its effects on the removal efficiency and the
treatment cost, keeping constant the other parameters (the initial temperature (θi) at 16.5 C°, the
stirring speed at 300 rev min-1, and the inter-electrode distance (d) at 2 cm). The pH, the
temperature, the difference in potential between the two electrodes and the final cadmium
concentration were measured for each sample. Also, the energy, electrodes consumption and
the treatment cost were calculated for each sample as a function of time. The characterization
and the treatment of the effluent were performed at the Water Treatment and Desalination
Research Unit of Tunis, Tunisia. The method of cadmium removal through EC used in this
study proved to be cost-effective.

2. 5. Treatment cost

The EC process required an operating cost which encompassed material (electrodes and
electrical energy) as well as other essential expenses consisting of sludge dewatering and
disposal. The low operating cost could be calculated as follows:

Operating cost = a C energy + b C electrode + D Eq. (6)

Where: (a) the energy cost: 0.2 (TND)/KWh; (b) the aluminum cost: 2. 8 Tunisian
National Dinar (TND) kg-1; C energy (kW h m-3) and C electrode (kg Al m-3) are consumption
quantities for the Cd (II) removal; D is cost of the chemicals used (D= cost of salt + cost acid =
0.1 TND m-3). Cost of electrical energy (kW h m-3) is calculated as:

UC × I × t
Cénergie (kWh / m 3 ) = Eq. (7)
V

Where U is the voltage cell (V), I is the current (A), t is the time of electrolysis (h) and V
is the volume (m3) of Cd (II) solution. Cost of electrode (kg Al m-3) is calculated by the
following equation according to Faraday’s Law:
6
 I ×t × M
Célectrodes (kg / m3 ) = Eq. (8)
n × F ×V

Where I is current (A), t is time of electrolysis (s), M is molecular mass of aluminum

(26.98 g mol-1), z is number of electron transferred (z = 3), F is Faraday’s constant (96487 C
mol-1) and V is volume (m3).

3- Results and discussion

3.1. Choice of electrode configuration

The EC efficiency is strongly related to the dissolution of the electrodes and the
production of a large amount of aluminum metal ions (Mollah et al. , 2001; Modirshahla et al. ,
2008), which is reinforced by an increase in the number of plates to get a larger active surface.
However, it is important to note that the number of plates should be increased in a way that
enables us to avoid the generation of a significant ohmic, and this depends on the type of
electrode configuration and the number of the electrodes used. Generally, we have two types of
electrode configuration (Fig. 2) where the number of the electrodes is varying between 4 and 8:
The first configuration is a monopolar electrode configuration, i.e. each electrode is connected
to either the anode or the cathode, and the second one is bipolar and thus involves connecting
only the first electrode to the anode and the last electrode to the cathode (Mamerie et al. , 1998;
Meunier et al. , 2004; Beauchesne et al. , 2005). In order to investigate the influence of electric
configuration and to choose one of the two configurations, two tests were carried out using 4
aluminum electrodes. The first test was done with a bipolar configuration, and the second one
with a monopolar configuration.

Table 2 shows that the electrode consumptions calculated through Eq. (8) above were
the same at each time interval, which could be explained by the fact that we had the same active
anode surface and the same current density in the same conditions, changing only the electrode
configuration. Electrode configuration, therefore, had no effect on the aluminum electrode
consumption. The obtained results presented in Fig. 3. support the hypothesis that increasing
the number of electrodes results in an increase in the removal efficiency. It was found that using
four electrodes made the treatment process much faster; 30 min to reach 90 % of cadmium
reduction, while 45 min were required if two electrodes were used for the same performance. It
is also clear from Fig. 3 and Table 2, that in the case of bipolar configuration cadmium
elimination was more efficient but required much energy and high cost if compared to
7
monopolar configuration. For the bipolar configuration, the removal efficiency reached 92%
and cost 0.55 TDN in 60 min of electrolysis time. However, for monopolar configuration, the
removal efficiency reached 87% and cost 0. 160 TND m-3 in 60 min. Thus, the choice of
monopolar configuration allowed high rate of removal efficiency negligibly lower than that
with bipolar configuration, and significant reduction in treatment cost. This result could be
explained by the fact that in bipolar connection there is a higher surface area resulting in more
anodic oxidation compared to that of monopolar connection. On the other hand, the increase of
the distance between the electrodes connected to DC current supply created an ohmic drop
relative to the anode and cathode voltages. This could be further explained through the
following equation:
d
R ohm = Eq. (9)
(S × k )
In the case of bipolar configuration, the increase in the inter-electrode distance resulted
in greater resistance to mass transfer and slower kinetics of charge transfer, which involved
much energy consumption as well as high cost (N. Meunier et al. , 2004; Khaoula et al. , 2013).
Therefore, based on the aforementioned results, the monopolar configuration had to be chosen
because of the high-rate removal efficiency it would yield with very low energy consumption
and cost.

3.2. Effect of the variation of the surface-area-to-volume ratio

3.2.1. Determination of the optimum S/V ratio

The surface-area-to-volume ratio S/V is an extremely important reactor design

parameter in EC. This ratio, whose unit of measurement is known as m-1, is the ratio of the
active surface area of the volume of the treated solution. According to the literature, the
increase in the ratio S/V results in the reduction of the current density consumption (Belhouta et
al. , 2010). Hence, it is made necessary to take into account this parameter and determine its
effect on the performance of the EC process. The effects of the variation of S/V on the cadmium
removal efficiency were studied by covering and deactivating either a part or all of the face of
each electrode using durable water-resistant sellotape. Fig. 4. shows a schematic view of the
electrodes covers.

EC tests were performed for the S/V ratio values: 3.4, 6.8, 10.2 and 13.6 m-1. As for the
width, it was the result of a compromise; it had to be large enough as required by the active
8
surface but it was limited by the width of the reactor to ensure homogeneity and constant
stirring of the solution. The variation of pH, difference in potential and energy consumption
versus time for the different values of the ratio S/V are summarized in table 3. Fig. 5. shows the
variation of the removal of cadmium over time for different values of the ratio S/V.

For the different values of ratio S/V studied, a percentage of cadmium removal of 99%
was achieved after 60 min, but there was a huge difference in terms of cost. As shown in table 3,
the larger was the S/V ratio, the much better were the removal efficiency and cost. An increase
in S/V ratio promoted the electrical transport, ensured better chemical dissolution of aluminum
and increased the resistance of the electrochemical cell. This resulted in an increasing removal
efficiency of cadmium by virtue of better chemical dissolution. The best cadmium removal
percentage as well as treatment cost was achieved for the S/V value of 13.6 m-1. Within 30 min
of electrolysis time, increasing the S/V value from 3.4 to 13.6 m-1 allowed an increase in
cadmium removal efficiency from 90.95% to 99.76% and a significant reduction in both
treatment cost from 1.130 to 0.280 TND m-3 and energy consumption from 10.2 to 1.75 KWh
m-3 proved by the decrease in the temperature of the solution from 21.1 to 18.4 °C. Thus, we
had to choose the largest S/V ratio possible. Accordingly, 13.6 m-1 was chosen as an optimum
value for the tests to significantly minimize the cost as well as electrolysis time and achieve
maximum removal.

3.2.2. Verification of Faraday's law as a function of S/V value

In order to verify Fraday’s law for the different S/V value studied and for an electrolysis
time of 30 min, the amount of aluminum oxide was theoretically calculated using Faraday's law
as follows:

..
é  Eq. (10)
.

Aluminum concentration was measured before and after each test to determine the mass
loss during each EC test. It should be noted that the experimental value is 80% of the faraday
efficiency. The experimental mass was determined by the following equation:


  

  
 Eq. (11)

The Faradic efficiency was calculated using the following equation:

9
 ೐ೣ೛೐ೝ೐೘೐೙೟ೌ೗
    100 Eq. (12)
೟೓೐೚ೝ೐೟೔೎ೌ೗

The experimental results are summarized in Table 4. The effect of current density on the
experimental evolution of the mass losses at the anode and cathode as well as those which were
theoretically expected according to Faraday's law is illustrated in Fig. 6.

Fig. 6 confirms that the theoretical mass was linearly proportional to the current density.
Meanwhile, the experimental mass varied in proportion to the applied current density, but it was
slightly higher than the theoretical mass. This resulted in a Faraday's efficiency above 100 %.
The evaluation of the Faradic yield of aluminum for various current densities is shown in Fig. 7.
The average Faradic efficiency obtained was 115.08 %. This result could be explained by an
anodic oxidation of the aluminum which simultaneously led to the formation of Al3+ and Al+
(Picard et al. , 2000). Similar to the results reported in previous studies, in the case of aluminum
configuration, 20% of the total electrode mass dissolved was due to chemical dissolution and
the remaining 80% by electrochemical dissolution (Anantha et al. , 2013). This difference in
valence directly affected the calculation of the theoretical mass dissolved. This consumption
may be also due to the chemical hydrolysis of the cathode according to the following equation:


2  6   2   2  3  Eq. (13)

In addition, this phenomenon could be explained by the phenomenon of corrosion and

oxidation of the surface of the electrodes. The mechanism of corrosion of the electrodes
suggested involvement of chloride ions. This mechanism can result in greater production of
aluminum hydroxide and hydrogen bubbles compared to the amount that is expected to produce
the main reaction at the anode (Secula et al. , 2012).

3.4. Effect of inter-electrode distance

To study the effect of the inter-electrode distance on the cadmium removal efficiency,
several EC tests were carried out for different inter-electrode distances of 0.5, 1 and 2 cm. The
variation of pH, difference in potential, temperature, and treatment cost and energy
consumption versus time for the different values of the S/V ratio are summarized in table 5.

When the inter-electrode distance increased, the ohmic loss in relation to the anode and
cathode over voltages and the resistance to mass transfer became larger; the kinetics of both
charge transfer and the aluminum oxidation was slowed down. Consequently, there was a
10
smaller amount of Al3+ cations at the anode leading to slower formation of coagulants in the
middle (Ghosh et al., 2008). The rate of particle aggregation and adsorption of cadmium
became lower, which explained the decrease in cadmium removal efficiency. This resulted in
lower removal efficiency at a larger inter-electrode distance.

Fig.8. and Table 5 clearly show that the removal percentages of Cd (II) decreased with
the increase of inter-electrode distance. The best cadmium removal percentage as well as
treatment cost was achieved for the inter-electrode distance value of 0.5 cm. Within 30 min of
electrolysis time, decreasing the inter-electrode distance from 2 to 0.5 cm resulted in an
increase in cadmium removal efficiency from 82.33% to 91.63% and a reduction in both
treatment cost (from 0.270 to 0.210 TND m-3) and energy consumption (from 0.87 to 0.55 KWh
m-3) which was clear from the decrease in the temperature of the solution from 19.5 to 17.8 °C.
This result proved that, unlike the case of electrode configuration and S/V ratio, the effect of the
inter-electrode distance on energy consumption and treatment cost was insignificant. On the
other hand, as the time progressed, it was clear that the formation of a gelatinous aluminum
hydroxide film on the anode developed a resistance that increased whenever the inter-electrode
distance increased. Hence, it was beneficial to choose an optimum short inter-electrode distance
of 0.5 cm to minimize energy consumption and increase the cadmium removal efficiency.

3.5. Effect of the initial water temperature

Temperature is one of the most important factors that can influence the cadmium
removal by EC (Chen, 2004; Koren and Syversen, 1995). To determine the optimum initial
temperature for the removal of cadmium through the EC process using two aluminum
electrodes, various EC tests were conducted for the different initial temperatures of 18, 30, 50
and 70 C°. The results obtained during testing the EC for different values of initial
temperature are reported in Table 5.

Fig. 9. illustrates the importance of the initial temperature in the removal efficiency of
cadmium from wastewater. It was found that with the increase in temperature and reduction of
electrolysis time the removal efficiency was significantly improved, but no difference was
made in terms of cost and energy consumption. In fact, due to the increase of the temperature,
the mass transfer increased and the kinetics of particle collision improved. Furthermore,
dissolution of the anode was improved and the amount of the hydroxide that was formed and
necessary for the adsorption of cadmium was greater at elevated temperature than when at low

11
temperature. In addition, a higher temperature allowed a production of larger hydrogen
bubbles, which increased the speed of flotation and reduced the adhesion of suspended particles
(Koren and Syversen, 1995). This is why the EC process needed to start with a high temperature
rather than heating the reaction. This allowed the removal efficiency to be improved. We found
that the yield was significantly improved with increasing the initial temperature of the solution,
which resulted in a reduction in the electrolysis time. As clearly shown in Fig. 9, the maximum
elimination of 98.28% was obtained for a temperature of θi = 50 C° and an electrolysis time of
30 min. Thus, the temperature of 50 °C was chosen as an optimum initial EC temperature on the
basis that it allowed the achievement of high removal efficiency in a short treatment time
especially because it did not made any change in the cost.

3.6. Effect of stirring speed

The effect of stirring speed was investigated in order to determine the influence of this
parameter on the cadmium removal efficiency by EC. To study the effect of the stirring speed,
EC was performed at different stirring speeds of 0, 300, 450 and 600 rev min-1. Results are
presented in table 6.

As shown in Fig. 10. the elimination of cadmium was much faster for a moderate
agitation speed. Adsorption is a phenomenon intrinsically very fast and essentially limited by
the mass transfer internally and externally. The cadmium elimination was low without
agitation; and the percentage of removal did not exceed 68 % for an electrolysis time of 30 min
and 80 % for an electrolysis time of 60 min. For a moderate agitation of 300 rev min-1, the
elimination was much faster than 0 rev min-1 and even further increased when the agitation was
up to 450 rev min-1 reaching a removal percentage of 95 %, 99.5 % after 30 and 60 min,
respectively. This proved that the adsorption of Cd (II) ions by the coagulant aluminum
hydroxide AlOH3 occurred very effectively for stirring speeds of 300 and 450 rev min-1.
However, there was a slight decrease in removal efficiency when the agitation reached 600 rev
min-1. This could be explained by the fact that excessive agitation resulted in the breaking of the
flocs. Moreover, the higher was the agitation, the more energy the agitator consumed and thus
required higher cost. Therefore, although moderate agitation speed of 300 rev min-1 had a
significantly positive effect on the removal efficiency, it made no difference at the level of
energy consumption and cost. This is why 300 rev min-1 was chosen as the optimum agitation
speed.

12
3.7. Investigation of the effect of all the optimum reactor design parameters on the removal of
cadmium from TCG industrial wastewater

In order to examine the effect of EC reactor design found in the present study on the
removal of cadmium from the TCG industrial wastewater under treatment, EC tests were
applied on this effluent after adjusting the pH at 7. The sample industrial wastewater collected
from the TCG contained a cadmium concentration of 2.83 mg L-1, a conductivity of 1.176 mS
cm-1 and an acid pH of 2.02. The physico-chemical characteristics of the case-study industrial
wastewater before and after the treatment are shown in Table 7. The pH, the temperature, the
energy consumption and the difference in potential between the two electrodes were measured
for each sample. The obtained results are summarized in Table 8.

As shown in Fig. 11, the testing of cadmium removal through the application of all the
selected optimum design parameters together was highly effective; it exceeded 100 % with a
very low power consumption of 1.6 kWh m-3 and very low cost of 0.116 TND m-3 in only 5 min.
Therefore, the time span chosen as an optimum parameter was 5 min. In this work, a
quantitative comparison was made between the obtained results of EC using optimum reactor
design parameters and results of precipitation and coagulation. The findings in this study
indicated that precipitation required 3.700 TND m-3, whereas coagulation, using AlCl3 as
coagulant, required 2.430 TND m-3 to remove the same quantity of cadmium from the
case-study wastewater. Thus, it is important to note that EC process using the selected optimum
design parameter proved to be highly efficient and, meanwhile, cost-effective; it enabled a
significant reduction in operating cost. The contribution of this study in terms of both efficiency
and cost can be further confirmed if we compare the cost of treatment process in previous study
(Oncel et al., 2013) where the operating costs at the optimum operating conditions were
determined to be 1.98 €
€ m3 (equivalent to 4.36 TND m-3) for EC and 4.53 €€ m-3 (equivalent to
9,96 TND m-3) for chemical precipitation.

3.8. Evolution of pH

As has been pointed out in several previous studies (Bayramoglu et al. , 2007; Daneshvar
et al. , 2006), the use of soluble anodes causes a change in the pH of the solution during EC. For
each EC parameter studied, the pH of the treated solutions was measured as a function of time.
As shown in tables. 2, 3, 5, and 6, the pH increased with increasing operating time. The final pH
depended on the type of electrodes configuration. For the same initial pH of 7, there was a large

13
variation in the final pH. As shown in table 2, after 60 min of electrolysis time, with bipolar
configuration the pH increased up to 10.90, whereas with the monopolar configuration the pH
increased up to 9.03. This result can be explained by the fact that the evolution of the final
solution pH depended on the buffer capacity (Eq.14) due to the production and consumption of
OH- ions during the EC (Eq.15), and thus avoided a sudden change in pH (Chen, 2004).

Al(OH)3 + OH- ↔ Al(OH)4- Eq. (14)

H 2O + 1 e - ↔ 1/2 H2 (g) + OH- Eq. (15)

5. Conclusion

The main objective of this study was to investigate the effect of reactor design
parameters on cadmium removal from industrial wastewater to improve as much as possible
efficiency and significantly reduce cost of EC process as well. Based on an examination of the
design parameters one by one, the selected parameters were: an inter-electrode distance of 0.5
cm, a monopolar connection mode, a surface-area-to-volume ratio (S/V) of 13.6 m-1, a
moderate agitation speed of 300 rev min-1, and an initial temperature of 50 °C. These operating
conditions were selected because they could simultaneously achieve efficient removal in a
relatively short operating time with the lowest energy consumption and cost possible. The
obtained results showed that the parameters under examination influenced removal efficiency.
However, the stirring speed and initial temperature do not have effect on energy consumption
and cost, while the S/V ratio, electrode configuration, inter-electrode distance make significant
change in terms of energy consumption as well as cost. The investigation of the effect of all the
selected EC design parameters together on the removal of cadmium from the wastewater
discharged by TCG proved that the treatment was highly effective; 100 % cadmium removal
was achieved in only 5 min, a very low power consumption of 1.6 kWh m-3 and very low cost of
0.116 TND m-3. Furthermore, EC was found to be able to remove cadmium as well as other
pollutants at the same time from the industrial wastewater under treatment. The investigation
carried out in this work explores and proposes a very cost-effective treatment method to remove
heavy metals from industrial wastewater if compared to results reported about cost of this
treatment process through other technologies used such as coagulation (4.36 TND m-3) and
precipitation (9,96 TND m-3) employed in previous studies. This treatment method is workable
for researchers seeking to achieve high-rate cadmium removal efficiency under similar
economic and operational conditions.
14
Acknowledgments

These research and innovation study have been carried out within the framework of a
MOBIDOC thesis funded by the European Union under the program PASRI. We greatly
appreciate the support of the TCG.

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18
Vasudevan, S., Lakshmi, J., 2011. Effects of alternating and direct current in electrocoagulation
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19
Fiig.11. Lab
boraatorry scaale celll asssem
mblly.

20
0
Fig. 2. Monopolar and bipolar electrode connection.

21
Fig. 3. Variation of residual cadmium concentration as a function of electrocoagulation
time (die= 2 cm, S/V= 13.6 m-1, θi= 16.5 C° and stirring speed 300 rev min-1).

22
Fig. 4. Schematic view of different electrodes covers in the EC process.

(d= 2cm, θi= 16.5 C° and stirring speed 300 rev min-1).

23
 Fig. 5. Variation of cadmium removal efficiency as a function of time for different
values of the S/V ratio (d= 2cm, θi= 16.5 C° and stirring speed 300 rev min-1).

24
 0.0045

0.004

0.0035

0.003

masse 0.0025
disoute (g) 0.002 m thé

0.0015 m exp

0.001

0.0005

0
3.4 6.8 10.2 13.6
S/V m-1

Fig. 6. Effect of S/V ratio on the anode consumption (d= 2cm, θi= 16.5 C° and stirring
speed 300 rev min-1).

25
 140

120
Rendement faradique (%)

100

80

60

40

20

0
0 2 4 6 8 10 12 14 16
S/V m-1

Fig. 7. Evolution of the faradic efficiency of aluminum as a function of S/V ratio (d=
2cm, θi= 16.5 C° and stirring speed 300 rev min-1).

26
Fig. 8. Effects of inter-electrode distance as a function of time on the Cd(II) removal
(S/V= 13.6 m-1, θi=16.5 C° and stirring speed 300 rev min-1).

27
Fig. 9. Effects of initial temperature as a function of time on the Cd (II) removal
(die= 2 cm, S/V= 13.6 m-1 and stirring speed 300 rev min-1).

28
 Fig. 10. Variation of cadmium concentration as a function of electrocoagulation
time for different agitation speeds (die= 2 cm, θi=16.5 C° and S/V= 13.6 m-1).

29
 3

2.5

resudual cadmium removed 2 with application of EC design parameters

without application of EC design parameters

1.5

0.5

0
0 10 20 30 40 50 60
time (min)

Fig. 11. Evolution of the residual cadmium removal with and without application
of reaction design parameters Vs time.

30
 Table.1. Results of the validation of the cadmium analysis by AASF.

Test Linearity Specificity Cochran Fidelity

CVr =
0.278;
Experiment Tobs = T’obs = CVR =
Fl = 2724 Fnl = 2.712 Cxobs = 0.498 0.170;
value 1.60 0.179 0.844
0.216;
0.118
C Cochran,
C Cochran, α=1%
Critic value VCl = 8.1 VCnl = 4.94 t (8; 0,995) = 3.355 α=5% = CVr < 5% CVR< 5%
= 0.721
0.629
No Point
The
The curvature Slope equal to 1 Origin group is Point group
Repeatable method is
Conclusion method and the and the method is considere is considered
Faithful Reprodctib
is Linear linearity is specific d no no suspect
le
approved aberrant

31
 Table. 2. Variation of pH, Temperature, difference between the potential, treatment cost,
electrodes consumption and energy consumption versus time for the different electric
configuration mode.
Treatment cost W Electrodes
tEC (min) θ (°c) pH U (V) (TND m-3) (KWh m-3) Consumption (Kg)

0 16.5 7.00 9.7 0.00 0.00 0.00

5 17 8.10 9.1 0.05 0.38 2.85 10-5

10 18 11.73 9 0.10 0.75 5.71 10-5

Bipolar
15 18 11.40 9 0.15 1.13 8.57 10-5
Configuration

30 19 10.95 8.8 0.29 2.20 1.71 10-4

45 20 10.80 8.7 0.43 3.26 2.57 10-4

60 21 10.90 8.3 0.55 4.15 3.43 10-4

0 16.5 7.00 3.6 0 0.00 0.00

5 16.5 8.32 2.6 0.01 0.11 2.85 10-5

10 17 8.14 2.5 0.03 0.21 5.71 10-5

Monopolar
15 18 8.08 2.5 0.04 0.31 8.57 10-5
Configuration

30 19 8.23 2.4 0.08 0.60 1.71 10-4

45 19 8.66 2.4 0.12 0.90 2.57 10-4

60 20 9.03 2.4 0.16 1.20 3.43 10-4

32
Table. 3. Variation of pH, difference between the potential, Temperature, treatment cost
and energy consumption versus time for the different values of the S/V ratio.
W Treatment cost
S/V (m-1) t(EC) (min) θ (°c) U (V) pH -3
(KWh m ) (TND m-3)
0 16.5 20.7 7.00 0.00 0.1
15 18.7 20.4 8.14 2.55 0.61
3.4 30 21.1 20.5 8.87 5.13 1.13
45 23.1 20.4 9.03 7.65 1.63
60 24.6 20.4 9.18 10.20 2.14
0 16.5 12.7 7.00 0.00 0.1
15 18.1 12.5 8.35 1.51 0.40
6.8 30 20.7 12.5 8.98 3.13 0.72
45 22.3 12.5 9.21 4.69 1.04
60 23.7 12.5 9.47 6.25 1.35
0 16.5 10.7 7.00 0.00 0.1
15 17.8 10.4 8.66 1.38 0.38
10.2 30 19.3 10.4 9.18 2.85 0.67
45 20.6 10.4 9.48 4.28 0.95
60 21.5 10.4 9.62 5.85 1.27
0 16.5 3.9 7.00 0.00 0.1
15 17.8 3.5 8.59 0.44 0.19
13.6 30 18.4 3.5 9.19 0.88 0.28
45 18.8 3.5 9.54 1.31 0.36
60 19.5 3.5 9.82 1.75 0.45

33
Table. 4. Effect of S/V value on the anode consumption and Faraday's efficiency.

S/V (m-1) 3.4 6.8 10.2 13.6

m theoretical(Kg) 0,00089 0,00176 0,002601 0,00329

m experimental(Kg) 0,00099 0,00199 0,002985 0,00398

R% Faradic 104.29 109.71 115.98 126.81

34
Table. 5. Variation of pH, difference between the potential, Temperature, treatment cost
and energy consumption versus time for the different values of inters-electrode distance.

W Treatment cost
die t(EC) (min) θ (°c) U (V) pH
(KWh m-3) (TND m-3)
0.1
0 16.5 2.3 7.00 0.00
0.152
15 17.2 2.1 8.58 0.26
0.21
0.5 30 17.8 2.2 9.20 0.55
0.264
45 18.6 2.2 9.39 0.82
0.32
60 19.0 2.2 9.48 1.10
0.1
0 16.5 3.0 7.00 0.00
0.162
15 17.6 2.5 8.35 0.31
0.224
1.0 30 18.7 2.5 8.78 0.62
0.288
45 19.5 2.5 8.95 0.94
0.35
60 20.6 2.5 9.13 1.25
0.1
0 16.4 3.9 7.00 0.00
0.188
15 18.6 3.5 7.82 0.44
0.274
2.0 30 19.5 3.5 8.14 0.87
0.362
45 20.7 3.5 8.16 1.31

60 21.2 3.5 8.32 1.75 0.45

35
Table. 6. Variation of pH, Temperature, difference between the potential, Treatment cost and
energy consumption versus time for different initial temperatures.

Treatment cost
θi (°c) t(EC) (min) θ (c°) U (V) pH W (KWh m-3)
(TND m-3)
0.1
0 18 2.3 7.00 0.00

0.1052
15 18.2 2.1 8.93 0.26

0.111
18 30 18.8 2.2 9.18 0.55

0.1164
45 19.6 2.2 9.36 0.82

0.122
60 20.0 2.2 9.41 1.10

0.1
0 30 3.0 7.00 0.00

0.1062
15 30.6 2.5 8.45 0.31

0.1124
30 30 31.8 2.5 8.70 0.62

0.1186
45 32.9 2.5 8.45 0.93

0.123
60 34.3 2.3 8.80 1.15

0.1
0 50 3.4 7.00 0.00

0.1082
15 48.3 3.3 7.56 0.41

0.1164
50 30 46.7 3.3 8.08 0.82

0.1246
45 45.4 3.3 8.28 1.23

0.133
60 42.8 3.3 8.96 1.65

0.1
0 70 3.9 7.00 0.00

0.1086
15 66.1 3.5 8.49 0.43
70
0.1174
30 63.2 3.5 8.70 0.87

0.1262
45 59.9 3.5 8.98 1.31

36
 0.135
60 57.2 3.5 9.49 1.75

Table. 7. Variation of pH, Temperature, difference between the potential, Treatment cost and
energy consumption versus time for different agitation speeds.
stirring speed W treatment cost
t(EC) (min) θ (c°) U (V) pH
(rev min-1) (KWh m-3) (DT m-3)
0 16.5 3.9 7.00 0.00 0.000

5 17.4 3.6 8.70 0.16 0.020

10 17.9 3.6 8.85 0.32 0.040

0 15 18.4 3.5 8.93 0.49 0.058

30 19.4 3.5 9.18 0.95 0.117

45 20.7 3.5 9.36 1.43 0.175

60 21.6 3.9 9.41 1.85 0.234

0 16.5 3.9 7.00 0.00 0.000

5 17.5 3.6 8.30 0.15 0.020

10 17.9 3.6 8.26 0.30 0.040

300 15 18.4 3.5 8.45 0.44 0.058

30 19.3 3.5 8.70 0.88 0.117

45 20.4 3.5 8.80 1.31 0.175

60 21.5 3.5 8.71 1.75 0.234

0 16.5 3.9 7.00 0.00 0.000

5 17.5 3.6 8.96 0.15 0.020

10 17.9 3.6 7.31 0.30 0.040

450 15 18.4 3.5 7.56 0.45 0.058

30 19 3.5 8.08 0.90 0.117

45 20 3.5 8.28 1.35 0.175

60 21 3.9 8.52 1.80 0.234

0 16.5 3.9 7.00 0.00 0.000

5 17.6 3.6 8.12 0.16 0.020

10 17.8 3.6 8.21 0.31 0.040

600
15 18.5 3.5 8.11 0.48 0.058

30 19.5 3.5 8.49 0.95 0.117

45 20.6 3.5 8.70 1.43 0.175

37
 60 21.5 3.9 8.98 1.90 0.234

Table. 8. Characteristics of the industrial wastewater before and after electrocoagulation

treatment.
Conductivit
θ [Cd2+] 2+
[Mg2+] [k+] [Na+]
pH y P2O5% MS % [Ca ] %
-1
(°C) % % % %
(mS cm )

Before
0.02
treatmen 2.02 1.176 15.0 0.49 0.025 0.02800 0.17 0.05 0.57
4
t

After
treatmen
10.94 1.158 18. 5 0.13 0.034 0.00029 0.07 0 0 0.13
t

38
Table. 9. Recording of the pH, the temperature, the energy consumption, the difference in
potential between the two electrodes as a function of time for the treatment of the
industrial wastewater.

Time (min) U (V) pH θ (c°) W (KWh m-3) Treatment cost

(TND m-3)

0 2.3 7.00 15.0 0.000 0.100

5 2.0 7.26 15.9 0.083 0.116

10 2.0 7.60 16.2 0.166 0.133

15 2.0 7.83 16.3 0.250 0.150

20 2.0 7.99 16.6 0.333 0.166

30 2.0 9.15 17.1 0.500 0.200

45 2.0 10.28 17.9 0.750 0.250

60 1.9 10.94 18.5 0.950 0.290

39
 Investigation of electrocoagulation reactor design parameters effect on the removal of
cadmium from synthetic and phosphate industrial wastewater

BRAHMI Khaled a, BOUGUERRA Wided a, HAMROUNI Béchir a, ALOUI Limam b, LOUNGOU Mouna c, Zied Tlili d
a U. R Traitement et Dessalement des Eaux, Département de Chimie,
Faculté des Sciences de Tunis, 2092 Manar II, TUNISIE, Tel./ Fax: +2167187128.
b U. R Matériaux, Environnement et Energie, Département de Chimie,
Faculté des Sciences de Gafsa, Campus Universitaire Sidi Ahmed Zarroug -2112 Gafsa, TUNISIE, Tel +216 76 211 026.
c Groupe Chimique Tunisien, Usine de M’Dhilla Gafsa, Km. 14 Route M’Dhilla- 2100 Gafsa, Tel +216 76211515.
d Higher Institute of Business Administration of Gafsa, Campus Universitaire Sidi Ahmed Zarroug -2112 Gafsa, TUNISIE, Tel +216 24951825.
Tel./ Fax: +21671871282; Corresponding author E-mail:khaled.brahmii@gmail.com

40