Journal of Hazardous Materials B112 (2004) 207–213

Treatment of electroplating wastewater containing Cu2+, Zn2+

and Cr(VI) by electrocoagulation
Nafaâ Adhoum∗ , Lotfi Monser, Nizar Bellakhal, Jamel-Eddine Belgaied
Centre Urbain Nord, Département de Chimie, Institut National des Sciences Appliquées et de Technologies, B.P. No. 676, 1080 Tunis Cedex, Tunisia

Received 15 September 2003; received in revised form 11 February 2004; accepted 2 April 2004

Abstract

The performance of electrocoagulation, with aluminium sacrificial anode, in the treatment of metal ions (Cu2+ , Zn2+ and Cr(VI)) containing
wastewater, has been investigated. Several working parameters, such as pH, current density and metal ion concentrations were studied in an
attempt to achieve a higher removal capacity. Results obtained with synthetic wastewater revealed that the most effective removal capacities
of studied metals could be achieved when the pH was kept between 4 and 8. In addition, the increase of current density, in the range
0.8–4.8 A dm−2 , enhanced the treatment rate without affecting the charge loading, required to reduce metal ion concentrations under the
admissible legal levels. The removal rates of copper and zinc were found to be five times quicker than chromium because of a difference in
the removal mechanisms. The process was successfully applied to the treatment of an electroplating wastewater where an effective reduction
of (Cu2+ , Zn2+ and Cr(VI)) concentrations under legal limits was obtained, just after 20 min. The electrode and electricity consumptions were
found to be 1 g l−1 and 32 A h l−1 , respectively. The method was found to be highly efficient and relatively fast compared to conventional
existing techniques.
© 2004 Elsevier B.V. All rights reserved.

Keywords: Electrocoagulation; Aluminium electrodes; Metal ions; Electroplating wastewater

1. Introduction at the ppm level [2]. Although, it is shown to be quite effec-

tive in treating industrial effluents, the chemical coagulation
Effluents issued from surface finishing and plating indus- may induce secondary pollution caused by added chemical
try usually contain, metal-ion concentrations much higher substances. This drawback, together with the need for low
than the permissible levels. Due to their high toxicity, indus- cost effective treatment, encouraged many studies on the use
trial wastewaters containing heavy metals are strictly reg- of electrocoagulation for the treatment of several industrial
ulated and must be treated before being discharged in the effluents.
environment. Various techniques have been employed for Electrocoagulation is a simple and efficient method where
the treatment of heavy metals, including precipitation, ad- the flocculating agent is generated by electro-oxidation of
sorption, ion-exchange and reverse osmosis. Precipitation is a sacrificial anode, generally made of iron or aluminium.
most applicable among these techniques and considered to In this process, the treatment is done without adding any
be the most economical [1]. It is based on chemical coagu- chemical coagulant or flocculant, thus reducing the amount
lation by adding lime to raise the pH and aluminium salt to of sludge which must be disposed [3]. The electrocoagula-
remove colloidal matter as gelatinous hydroxides. Activated tion has been successfully used to treat oil wastes, with a
silica or polyelectrolytes may also be added to stimulate removal efficiencies as high as 99% [4,5]. A similar success
coagulation. The former treatment may be followed by ad- was obtained when treating dye-containing solutions [6–8],
sorption onto activated carbon to complete metals removal potable water [9], urban and restaurant wastewater [10,11]
and nitrate or fluoride containing waters [12,13]. In addition,
a great deal of work performed in the last decades [14–17]
∗ Corresponding author. Tel.: +216 1 703627; fax: +216 1 704329. has proved that electrocoagulation is an effective technology
E-mail address: [email protected] (N. Adhoum). for the treatment of heavy metal containing solutions.

0304-3894/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2004.04.018
208 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213

In the present work, the efficiency of electrocoagulation in When a real industrial wastewater was treated, the de-
removing copper, zinc and chromium from wastewater of an crease of chemical oxygen demand (COD) was measured,
electroplating unit was reported. The effect of the wastewater using a COD reactor and direct reading spectrophotometer
characteristics, initial pH and metal-ion concentrations and (Beckman model DU 530).
operational variables, current density and treatment time, on
the removal efficiency is explored and discussed to deter-
mine the optimum operational conditions. The optimum op- 3. Brief description of electrocoagulation mechanism
erational parameters were used for wastewater treatment of
a local electroplating unit. Electrocoagulation is based on the in situ formation of the
coagulant as the sacrificial anode corrodes due to an applied
current, while the simultaneous evolution of hydrogen at the
2. Experimental details cathode allows for pollutant removal by flotation. This tech-
nique combine three main interdependent process, operating
2.1. Reagents synergistically to remove pollutants: electrochemistry, coag-
ulation and hydrodynamics. An examination of the chemical
The electrodes used in this study consisted of aluminium reactions occurring in the electrocoagulation process shows
plates (100 mm × 50 mm × 0.5 mm) of 99% purity, pur- that the main reactions occurring at the electrodes are:
chased from Prolabo, France. All other chemicals were of
Al
Al3+ + 3e (anode) (1)
analytical grade and supplied by Fluka, France. Stock syn-
−
thetic wastewater solutions of 800 mg l−1 chromium, cop- 3H2 O + 3e
3
2 H2 + 3OH (cathode) (2)
per or zinc were, respectively, prepared by dissolving the
required amounts of potassium dichromate, copper sulphate In addition, Al3+ and OH− ions generated at electrode
or zinc sulphate in water. Solutions of lower concentrations surfaces react in the bulk wastewater to form aluminium
were prepared by proper dilution. hydroxide:
The pH of the solution was adjusted to the required value Al3+ + 3OH−
Al(OH)3 (3)
with 10−2 M hydrochloric acid and 10−2 M sodium hydrox-
ide. If the anode potential is sufficiently high, secondary reac-
All measurements were carried out at ambient temper- tions may occur at the anode, such as direct oxidation of or-
ature (25 ± 1 ◦ C), on 200 ml aliquots of synthetic or real ganic compounds and of H2 O or Cl− present in wastewater:
industrial wastewater (collected from an electroplating 2Cl−
Cl2 + 2e (4)
unit) added with the same amount of potassium chloride
+
(0.74 g) to avoid excessive ohmic drop and to limit the 2H2 O
O2 + 4H + 4e (5)
formation of the passivation layer on aluminium elec- The produced chlorine undergoes a dismutation reaction
trodes. As has been shown in previous study [18], the at pH higher than 3–4:
addition of halide salts will decrease the energy consump-
tion and limit the temperature variations, due to the Joule Cl2 + H2 O
HClO + H+ + Cl− (6)
effect. HClO
ClO + H − +
(7)
2.2. Electrocoagulation procedure The aluminium hydroxide flocs act as adsorbents and/or
traps for metal ions and so eliminate them from the solution.
Electrocoagulation was carried out in a 250 ml beaker Furthermore, a direct electrochemical reduction of Cr(VI)
without stirring, using three parallel aluminium electrodes in Cr(III) may occurs at the cathode surface [3,16,19]. Si-
spaced by 5 mm and dipped in the wastewater. A radiometer multaneously, the hydroxyl ions which are produced at the
potentiostat/galvanostat of the type DEA 332 interfaced to cathode, increase the pH in the electrolyte and may induce
an IBM personal computer was used in galvanostatic mode coprecipitation of Cu2+ , Zn2+ and Cr(III) in the form of
to supply a constant current. The electrodes were connected their corresponding hydroxides [3,4,9]. This acts synergis-
in such a manner that the central electrode functioned as a tically to remove pollutants from water.
sacrificial anode (active surface = 50 cm2 ), while the two
others operated as cathodes.
To follow the progress of the treatment, samples of 2 ml 4. Results and discussion
were periodically taken from the reactor then filtered to elim-
inate sludge formed during electrolysis. The residual con- The electrocoagulation process is quite complex and may
centrations of metal ions were determined by atomic absorp- be affected by several operating parameters, such as pollu-
tion spectrophotometer (Perkin–Elmer, model Analyst 300). tants concentrations, initial pH and current density. In order
At the end of the experiment, the solution was filtered and to enhance the process performance, the effects of those pa-
the precipitate was dried and weighed. rameters have been explored.
 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213 209

105
Cu
95 Zn
Cr
Removal efficiency / %

85

75

65

55

45

35
0 2 4 6 8 10
Initial pH

Fig. 1. Effect of initial pH on metal ions removal. Initial concentrations of Cu2+ , Zn2+ and Cr(VI) = 50 mg l−1 each, j = 1.6 A dm−2 , anode surface
= 50 cm2 , time of electrolysis = 20 min.

4.1. Effect of initial pH observed (58%), while removal yields of Cu2+ and Zn2+
remained very high. Furthermore, it can be seen that the re-
It has been established that the initial pH [8,11] has a con- moval efficiency of all studied ions decreased significantly
siderable influence on the performance of electrocoagulation upon decreasing initial pH. Removal yield lower than 55%
process. To evaluate its effect, a series of experiments were was achieved at pH 2. The decrease of Re at a pH less than
performed, using solutions containing a mixture of Cu2+ , 4 and higher than 8 was observed by many investigators
Zn2+ and Cr(VI) of 50 mg l−1 each, with an initial pH vary- and was attributed to an amphoteric behaviour of Al(OH)3
ing in the range 2–10. which lead to soluble Al3+ cations, when the initial pH is
As illustrated in Fig. 1, the removal efficiencies (Re ) of low and to monomeric anions Al(OH)4 − , when the initial
copper and zinc, after 15 min of electrolysis at 0.8 A, reached pH is high [8]. These soluble species are useless for water
value as high as 99.9%, when pH exceed 4. In the same treatment. When the initial pH was kept in the range 4–8, all
conditions, the removal yield of chromium reached a max- aluminium cations produced at the anode formed polymeric
imum of about 83% and seemed to be not affected by pH, species Al13 O4 (OH)24 7+ [20,21] and precipitated Al(OH)3
as long as this later is kept in the range between 4 and 8. leading to a more effective treatment. The high efficiency of
In contrast, when the initial pH is increased above 8, a dra- Cu and Zn removal, even at a high pH, might be ascribed to
matic decrease of the removal efficiency of chromium is the precipitation of their hydroxides at the cathode, which

10

8
Final pH

3
0 2 4 6 8 10
Initial pH

Fig. 2. pH variation after electrocoagulation. Initial concentrations of Cu2+ , Zn2+ and Cr(VI) = 50 mg l−1 each, j = 1.6 A dm−2 , anode surface = 50 cm2 ,
time of electrolysis = 40 min.
210 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213

start at pH ∼ 6–7 for copper and ∼ 7–8 for zinc. At alka- 100
-1

j = 4.8 A dm-2
Residual Cu concentration/mg l

line pH between 8 and 10, dichromate ions are converted to

soluble chromate (CrO4 2− ) anions, which goes some way j = 3.2 A.dm-2
j = 1.6 A.dm-2
towards explaining its less effective removal. 10
j = 0.8 A.dm-2
As observed by other investigators [9,11], the treatment
induced an increase in the pH when the initial pH was low
2+

(between 2 and 9) as shown in Fig. 2. This might be ex- 1

plained by the excess of hydroxyl ions produced at the cath-
ode in sufficiently acidic conditions and by the liberation
of OH− due to the occurrence of a partial exchange of Cl−
with OH− in Al(OH)3 [11]. When the initial pH is above
0.1
0 5 10 15 20 25 30
9, the formation of Al(OH)4 − species together with parasite (a) Time/min.
attack of the cathode by hydroxyl ions [18] lead to a slight 100
decrease in the pH.
-1

j = 4.8 A.dm-2
Residual Zn concentration/mg l

As a result of the previous discussion of the effect of pH j = 3.2 A.dm-2

on the removal efficiency, the initial pH was adjusted to 6 10 j = 1.6 A.dm-2
for all subsequent studies. j = 0.8 A.dm-2

1
4.2. The effect of current density
2+

0.1
The current density not only determines the coagulant
dosage rate, but also the bubble production rate and size
[21,22]. Thus, this parameter should have a significant im- 0.01
0 5 10 15 20
pact on pollutants removal efficiencies. (b) Time/min.
To investigate the effect of current density and charge
100
loading on the removal yield, a series of experiments were
Residual Cr(VI) concentration/mg.l -1

j = 4.8 A.dm-2
carried out on solutions containing a constant pollutants j = 3.2 A.dm-2
loading with current density being varied from 0.8 to j = 1.6 A.dm-2
4.8 A dm−2 . Fig. 3 is a semi-logarithmic plot, showing the 10 j = 0.8 A.dm-2

normalised concentrations profiles of the studied metal ions

for typical electrocoagulation runs, where the initial pH
was fixed at 6. The removal rate of all studied metal ions 1
increased upon increasing current density. The highest cur-
rent (4.8 A dm−2 ) produced the quickest removal rate, with
a 96% concentration reduction occurring just after 10 min. 0.1
0 10 20 30 40 50
This expected behaviour is easily explained by the increase (c) Time/min.
of coagulant and bubbles generation rate, resulting in a more
efficient and faster removal, when the current is increased Fig. 3. Effect of current density on the removal rate of Cu2+ (a), Zn2+
[21,23]. Indeed, the amounts of aluminium and hydroxide (b) and Cr(VI) (c) initial concentrations of Cu2+ , Zn2+ and Cr(VI)
= 50 mg l−1 each, anode surface = 50 cm2 .
ions generated at a given time, within the electrocoagula-
tion cell are related to the current flow, using Faraday’s
law:
ItM To optimise the treatment efficiency, optimum charge load-
m= (8) ing required to achieve high removal yields (residual con-
zF
centration under 2 mg l−1 ) for each metal ion, were cal-
where I is the current intensity, t is the time, M is the molec- culated at different current densities. The results shown in
ular weight of aluminium or hydroxide ion (g mol−1 ), z is Fig. 4, pointed out that the removal rate of zinc is almost
the number of electrons transferred in the reaction (3 for two times faster than that of copper and five times faster
aluminium and 1 for hydroxide) and F is the Faraday’s con- than chromium. Indeed, the volumetric electrical charges en-
stant (96486 C mol−1 ). suring 96% removal of zinc and copper were, respectively,
Moreover, it was previously shown that the bubble size 9 and 17.4 mF l−1 , while that needed to achieve the same
decreases with increasing current density [22], which is ben- removal efficiency of chromium was 59.4 mF l−1 . Further-
eficial to the separation process. Nevertheless, as the time more, as observed by other investigators [21,23], a slight
progresses, the amount of oxidised aluminium and the re- increase of charge loading is observed for chromium, when
quired charge loading increase. However, these parameters current density was varied in the range 0.8–4.8 A dm−2 . At
should be kept at low level to achieve a low-cost treatment. high current, the bubble density and upwards flux increased
 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213 211

0.07
Cu2+

0.06 Zn2+
Cr(V I)

0.05
-1
Charge loading/F l

0.04

0.03

0.02

0.01

0
0 1 2 3 4 5
-2
Current density/A dm

Fig. 4. The effect of current density on charge loading. Initial concentrations of Cu2+ , Zn2+ and Cr(VI) = 50 mg l−1 each, anode surface = 50 cm2 .

and resulted in a faster removal of the coagulant by flotation. 4.3. The effect of metal ion concentration
Hence, there is a reduction in the probability of collision
between the coagulant and pollutants. Nevertheless, when In order to examine the effect of metal ion concentration
Cu2+ or Zn2+ are considered, the required charge loading present in the wastewater on the removal rate, several solu-
are not affected by current. The differences of behaviour and tions containing increased concentrations (50–800 mg l−1 )
removal rates between Cu2+ , Zn2+ and Cr(VI) could be at- of Cu2+ , Zn2+ and Cr(VI) were treated and the residual
tributed to a difference in the removal mechanisms. Indeed, concentrations of ions were measured at different times of
coprecipitation of Cu(OH)2 and Zn(OH)2 may play a dom- electrolysis.
inant role in the removal mechanism of the corresponding Fig. 5 shows the change in the removal rate of zinc with
metallic ions. Regardless the slight increase (below 20%) of initial concentration. Copper and chromium removal rates
the charge loading observed for Cr(VI), the time required showed the same trends. As expected, it appears that the re-
to achieve the treatment can be shortened by a factor of six, moval rate has decreased upon increasing initial concentra-
when current density is increased from 0.8 to 4.8 A dm−2 , tion. This induced a significant increase of charge loading
while the cost of the treatment remained unchanged. Hence, required to reach residual metal concentrations below the
the highest current should be selected to obtain the quickest levels admissible for effluents discharged into the sewage
removal rate. system (2 mg l−1 ), as shown in Fig. 6. It can be observed that

450
initial 50 mg/l Zn2+
400 initial 100 mg/l Zn2+
-1
Residual Zn concentration/mg l

350 initial 200 mg/l Zn2+

initial 400 mg/l Zn2+
300

250

200
2+

150

100

50

0
0 10 20 30 40 50
Time/min.

Fig. 5. The effect of initial concentration on the removal efficiency of zinc ions. j = 4.8 A dm−2 , anode surface = 50 cm2 .
212 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213

500
Zinc
450
Copper
-1
Volumetric charge loading/mF l

400 Chromium

350

300

250

200

150

100

50

0
0 100 200 300 400 500
-1
Initial concentration/mg l

Fig. 6. The effect of initial concentration on the charge loadings required for an effective removal of Zn2+ , Cu2+ and Cr(VI) j = 4.8 A dm−2 , anode
surface = 50 cm2 .

charge loading undergo a linear increase with initial con- ried, using a wastewater sample, collected from an electro-
centration. This result proves that the amount of aluminium plating unit and the residual concentrations of Cu2+ , Zn2+
delivered per unit of pollutants removed is not affected by and Cr(VI) together with COD were measured at different
the initial concentration. In addition, the charge loading re- times of electrolysis.
quired to remove chromium to the admissible level, is much The initial concentrations of Cu (33 mg l−1 ), Zn
higher than that required for Cu2+ and Zn2+ . This confirmed (41 mg l−1 ) and Cr (24 mg l−1 ) were shown to exceed the
the less efficient removal of chromium compared to copper prescribed legal limits. In addition, the COD content of the
and zinc and indicated that longer electrolysis time is nec- wastewater (302 mg l−1 ) was found to be more than two
essary for chromium removal. Indeed, at high initial con- times the authorised limit, indicating the presence of some
centration (200 mg l−1 ), zinc and copper were reduced to organic compounds which were added to the electroplating
admissible levels after only 15 min. However, 1 h was nec- bath as brighteners, levellers or wetting agents.
essary to achieve the efficient removal of chromium. It appears from the results shown in Fig. 7 that the resid-
ual concentrations of copper and zinc were rapidly reduced
4.4. Treatment of an industrial wastewater under the legal limits, just after 5 min. Whereas, the resid-
ual concentration of chromium decreased more slowly and
To validate the suitability of electrocoagulation for the reached 2 mg l−1 after an electrolysis time of 20 min. The
treatment of industrial wastewater, an electrolysis was car- removal rates of metal ions seems to be relatively slow

50
COD/7
45
Cu2+
40 Zn2+
Cr(V I)
35
-1
Concentration/mg.l

30

25

20

15

10

0
0 5 10 15 20 25 30 35 40
Time/min.

Fig. 7. Effect of electrolysis time on the residual concentrations and COD content. j = 4.8 A dm−2 , anode surface = 50 cm2 .
 N. Adhoum et al. / Journal of Hazardous Materials B112 (2004) 207–213 213

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