Environmental Technology

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Treatment of galvanic effluent through

electrocoagulation process: Cr, Cu, Mn, Ni removal
and reuse of sludge generated as inorganic
pigment

Bruno Matheus Favero, Ana Carolina Favero, Daniela Coelho da Silva,

Patricia Hubner, Fernanda Siqueira Souza & Janice Botelho Souza Hamm

To cite this article: Bruno Matheus Favero, Ana Carolina Favero, Daniela Coelho da Silva, Patricia
Hubner, Fernanda Siqueira Souza & Janice Botelho Souza Hamm (2021): Treatment of galvanic
effluent through electrocoagulation process: Cr, Cu, Mn, Ni removal and reuse of sludge generated
as inorganic pigment, Environmental Technology, DOI: 10.1080/09593330.2021.1916089

To link to this article: https://doi.org/10.1080/09593330.2021.1916089

Published online: 21 Apr 2021.

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ENVIRONMENTAL TECHNOLOGY
https://doi.org/10.1080/09593330.2021.1916089

Treatment of galvanic effluent through electrocoagulation process: Cr, Cu, Mn, Ni

removal and reuse of sludge generated as inorganic pigment
Bruno Matheus Faveroa, Ana Carolina Faveroa, Daniela Coelho da Silvab, Patricia Hubnerc, Fernanda
Siqueira Souzaa and Janice Botelho Souza Hamma
a
Master in Environmental Impact Assessment, La Salle University, Canoas, Brazil; bLaboratory of Soil Analysis, Federal University of Rio Grande
do Sul, Porto Alegre, Brazil; cAnalytical Centre of Chemical Engineering Department, Federal University of Rio Grande do Sul, Porto Alegre,
Brazil

ABSTRACT ARTICLE HISTORY

Galvanic effluents are composed of a wide range of heavy metals, requiring adequate treatment to Received 26 September 2020
remove these contaminants and to meet the limits established by environmental agencies. Accepted 5 April 2021
Considering this aspect, the present study had as main objectives: (i) to evaluate the efficiency
KEYWORDS
of the electrocoagulation (EC) in the treatment of a galvanic effluent, with the purpose of Electrocoagulation; iron
removing total Cr, Cu, Mn, Ni and (ii) reuse the sludge generated for inorganic pigment electrodes; inorganic
production. EC tests were carried out through factorial design 23 with triplicate central point. pigment; sludge reuse;
pH (3, 7, 11), reaction time (15, 22.5 and 30 min) and current density (10, 17.5 and 25 mA/cm2) heavy metals removal
were the control variables. Under ideal experimental conditions (pH 7.00; t = 22.5 min and DC =
17.5 mA/cm2) were removed 96.94% of Mn, 97.63% of Cu and 99.99% of total Cr and Ni,
allowing to meet the limits provided in CONAMA Resolution 430/2011. The production of
inorganic pigments from a mixture of 10% sludge (generated in the ideal experimental
condition) and Al2O3 and TiO2 proved to be technically viable. It was obtained 8.27 g of a
brown inorganic pigment, composed mainly of Al1.82Cr0.18O3, Ca0.999(Ti0.805Fe0.201)O2.899 and
Fe2.18O4Ti0.42. Therefore, the results obtained demonstrate that EC is an effective technique in
galvanic effluents treatment. The sludge generated in this process showed to be appropriated
to be reused in inorganic pigment production and could be considered as an alternative to
reduce the environmental impact related to electroplating process.

CONTACT Bruno Matheus Favero bmfavero@gmail.com Master in Environmental Impact Assessment, La Salle University, Victor Barreto Ave., 2288,
Canoas, Rio Grande do Sul 92010-000, Brazil
© 2021 Informa UK Limited, trading as Taylor & Francis Group
2 B. M. FAVERO ET AL.

Introduction Overall reaction:

Electroplating is an industrial process characterized on 4Fe(s) + 10H2 O(l) + O2(g)
4Fe(OH)3(s) + 4H2(g) (8)
the deposition of a fine layer of one metal on another
metal or material through electrolytic process, to
After the formation of Fe(OH)2 and Fe(OH)3 coagu-
provide the surface of the manufactured product with
lants (through mechanisms I and II), the successive
various properties and attributes, such as corrosion pro-
stages of destabilization of contaminants, suspending
tection, enhanced surface hardness, colour, aesthetics
particles and breaking of emulsions begin; and the
and value addition [1,2]. This activity involves alkaline
aggregation of the destabilized phases to form flocs
cleaning, acid pickling, plating, and rinsing and as such
[14], allowing heavy metals removal.
generate large volume of untreated wastewater [3,4].
EC process inherits the advantages of classic chemical
Due to its composition, that include a wide variety of
coagulation (CC) and overcomes many key problems in
heavy metals [5], electroplating wastewater is con-
its practical application such as large sludge production
sidered extremely toxic.
and high operating cost [15]. According to Govindan
With greater quantities of wastewater being pro-
et al. [16], the EC process does not require the addition
duced, and increasingly stringent regulations governing
of chemicals and is characterized by the ease operation,
wastewater discharge, there is a growing need for more
short reactive retention time and low operational cost,
efficient and cost effective methods to remove heavy
being considered an economic treatment when com-
metals [6]. In this context, electrocoagulation (EC) has
pared to CC, according to the studies by Bayramoglu
been identified in recent studies as a promising tech-
et al. [17] and Akbal and Camci [18]. Bayramoglu et al.
nique for removing heavy metals such as Cd, Cr, Cu,
[17] carried out the treatment of a textile wastewater
Fe, Ni and Zn, contained in effluents from different
through EC (with iron electrodes) and CC (using FeCl3.-
sources [7–11]. EC method is based on the application
6H2O and Fe2(SO4)3.7H2O coagulants) with costs of
of a potential difference in the sacrifice electrodes,
0.25 $/m3 (EC) and 0.67 and 0.75 $/m3 (CC). Akbal and
which favours anode oxidation reactions (metallic ion
Camci [18] identified that the operating costs of a
dissolution into the aqueous medium) and cathode
metal plating effluent treatment through EC (with iron
reduction (formation of OH− ions and H2 gas). For iron
electrodes) and CC (using FeCl3 coagulant) were,
electrodes, reactions that occur at the anode and
respectively, US$ 0.59/m3 and US$ 0.86/m3.
cathode can develop through two mechanisms,
Despite the benefits of the EC technique, there are
described in Equations (1)–(8) [12,13].
several key parameters that influence the performance
Mechanism I:
of this process efficiency in removing metal ions [19].
Anode:
According to Hakizimana et al. [20], operating conditions
− (such as current, operation time, wastewater pH, alka-
Fe(s)
Fe2+
(aq) + 2e (1)
linity, conductivity, among others) affect EC effective-
− ness, and should be considered when applying this
(aq) + 2OH(aq)
Fe(OH)2(s)
Fe2+ (2)
process. The analysis of the interactions between the
Cathode: operational parameters has been carried out through
experimental design methodologies, to discover an
2H2 O(l) + 2e−
2OH−
(aq) + H2(g) (3) optimum operating condition with a minimum
number of tests [8]. In this context, factorial design of
Overall reaction:
experiments has been extensively used to process devel-
Fe(s) + 2H2 O(l)
Fe(OH)2(s) + H2(g) (4) opment and optimization because it allows the simul-
taneous analysis of the effects of many process
Mechanism II: variables at different levels as well as their interactions
Anode: [21]. Recent studies have applied experimental design
− methodologies to real or artificial industrial effluents
4Fe(s)
4Fe2+
(aq) + 8e (5)
treatment, either through electrocoagulation [22–24]
+
or through other techniques, such as adsorption/bio-
(aq) + 10H2 O(l) + O2(g)
4Fe(OH)3(s) + 8H(aq)
4Fe2+ (6) sorption [25–27].
The sludge generated after the treatment of galvanic
Cathode:
effluents through EC process is classified as a Class I
8H+ −
(aq) + 8e
4H2(g) (7) hazardous waste, according to NBR 10004 [28], which
prevents its direct disposal in the environment. As a

result, it is necessary to dispose this sludge in licensed
landfills, generating extra costs for industries and
making it impossible to reuse the metals contained
therein. An alternative for the reuse of galvanic sludge
is the production of inorganic pigments, substances
that develop colour in organic solids such as ceramics
and glazes, and are usually a complex mixture of
oxides, and relatively low-cost [29]. Studies have
shown that the use of galvanic sludge in the production
of inorganic pigments is feasible, obtaining pigments
with a pattern similar to the industrial one [30,31].
Further research required for EC treatment process
involve more extensive studies in the fields of process
optimization, modelling, scale up and process inte-
gration, in order to prove the reliability of this technol-
ogy for efficient large scale wastewater treatment [19].
The efficiency of the EC technique in the treatment of
galvanic effluents has been demonstrated in recent
studies [9,32,33]. However, few studies address in the lit-
erature the simultaneous removal of Cr, Cu, Mn and Ni
from a real and concentrated galvanic effluent, using
the EC method (with iron electrodes), as well as the
proposition of an alternative for the reuse of solid
waste generated in the EC process. In this context, the
present study had as main objectives: (i) to evaluate
the efficiency of the EC process in the treatment of a gal-
vanic effluent, in order to remove total Cr, Cu, Mn, Ni and
(ii) reusing the sludge generated in the EC process as an
inorganic pigment.
Materials and methods
Effluent
Raw galvanic effluent evaluated in this study was gener-
ated from chrome plating spent baths, performed by a
metal-mechanic industry located in the south of Brazil.
The effluent was kept in a closed plastic gallon (15 L),
at room temperature (9–15°C) during the tests.
Electrocoagulation tests (EC) and experimental
design
Electrocoagulation tests (EC) were carried out at room
temperature, using 950 mL of raw effluent and an EC
system that consisted of a DC source (0–25 V and 0–5
A) (MMECL, 6028), a reactor (15-cm diameter, 14 cm
height), four iron electrodes (dimensions 7.3 × 0.3 ×
7.5 cm) and a magnetic stirrer (Fisatom, 752 A).
Effluent pH and conductivity were monitored (before
and after each EC test) using a pH meter (Hanna, HI
8424) and a conductivity meter (Oakton, WD-35607-
10), previously calibrated.
ENVIRONMENTAL TECHNOLOGY 3
Experimental conditions of the EC tests were estab-
lished through factorial design 23 with triplicate central
point. Control variables were pH (3, 7 and 11), reaction
time (t) (15, 22.5 and 30 min) and current density (DC)
(10, 17.5 and 25 mA/cm2), chosen according to the adap-
tation of the methodology proposed by El-Taweel et al.
[34], Khan et al. [35] and Vignesh et al. [6], respectively. 1
mol/L H2SO4 (Neon) and 1 mol/L NaOH (Dinamica) were
used to initial pH adjustment. The response variables
obtained were the removal percentages of total Cr, Cu,
Mn and Ni, determined after the analysis of treated
effluent samples. Pareto graphs were obtained using
Statistica® 10.0 software. Statistical validation of the
results was performed through ANOVA test (95% confi-
dence level).
Determination of total Cr, Cu, Mn and Ni
concentrations
Total Cr, Cu, Mn and Ni concentrations in raw and
treated effluent were determined through the 3120 B
method (ICP – Plasma Inductively Coupled), using an
optical emission spectrometer with inductively coupled
plasma (Agilent, 710 Axial) and nitric-perchloric diges-
tion of the samples [36], with HClO4 (Moderna) and
HNO3 (Anidrol). Removal percentages were calculated
according to Equation (9).
[Ci ] − [Cf ]
Removal(%) = × 100 (9)
[Ci ]
where [Ci] is the initial concentration and [Cf] represents
the final concentration of the chemical element in the
sample.
Production of inorganic pigments
Inorganic pigment was produced in brown colour, using
10% galvanic sludge (obtained in the ideal treatment
condition). The sludge was previously oven dried
(Quimis, model Q-314.D242), at 150°C, for a period of
12 h. Drying temperature was based on the method-
ology presented by Jose et al. [37]. 44.1% of Al2O3 and
45.9% of TiO2 were added to the sludge, according to
an adaptation of the methodology proposed by Un
et al. [38]. The mixture was homogenized with the
addition of a small volume of distilled water and after
calcined in an oven (Quimis, model Q318M21) at 1100°
C for 2 h, according to the adaptation of the method-
ology of Sangwong et al. [39]. After cooling, the calcined
material was pulverized and analysed through X-ray
diffraction (XRD) and scanning electron microscopy
(SEM) techniques.
The test for colour fixing was performed according to
the methodology proposed by Un et al. [38], through the
mixture of transparent glaze (Vitro 150°, Acrilex) and the
4 B. M. FAVERO ET AL.

Table 1. Characterization of raw galvanic effluent. galvanic sludge and pigment was observed by SEM tech-
Parameter Raw effluent nique, from the cross section and surface obtained in a
Al (mg/L) 16.29 scanning electron microscope (Phenom World, PRO X).
As (mg/L) <2.00
Ba (mg/L) 4.48
Cd (mg/L) 0.47
Ca (mg/L) 336.77 Results and discussion
Pb (mg/L) 2.15
Co (mg/L) 1.51 Characterization of raw effluent
Cu (mg/L) 25.29
Conductivity (mS/cm) 12.54
Cr (mg/L) 4989.42
The results obtained after raw effluent characterization
S (mg/L) 177.92 are shown in Table 1.
Fe (mg/L) 3085.79 Raw galvanic effluent presented high concentrations
P (mg/L) 6.33
Mg (mg/L) 283.48 of total Cr (4989.42 mg/L), Ni (3560.09 mg/L) and Fe
Mn (mg/L) 130.65 (3085.79 mg/L). Other chemical elements (such as Al,
Ni (mg/L) 3560.09
pH 2.70 Ca, Cu, S, Mg, Mn, Na and Zn) were also identified in con-
K (mg/L) 4.95 siderable concentrations in the aqueous medium,
Se (mg/L) <4.00
Na (mg/L) 448.88 demonstrating the high polluting load of the analysed
V (mg/L) <0.20 effluent.
Zn (mg/L) 14.21

Electrocoagulation tests (EC)

pigment produced, in a proportion of 5% wt. The
mixture was applied on a tile and remained at rest for
24 h, for drying at room temperature. After this period,
the tile was dried at 150 °C for 30 min.
Characterization of galvanic sludge and inorganic
pigment
Galvanic sludge and the inorganic pigment produced
were analysed through XRD technique, using a diffract-
ometer (X’Pert Philips, MDP) with a CuKα radiation
source (λ = 1,542 Å). Diffractograms were obtained in
the range of 5–75° in 2θ, with a step of 0.05°/1 s.
Match!® v.3.9.0.158 software was used to confirm the
diffraction peaks and the crystalline structures observed.
The experimental results were compared to the crystal-
lographic information cards available in the Crystallogra-
phy Open Database [40]. The morphology of the
Figure 1 shows the removal percentages obtained for
total Cr, Cu, Mn and Ni after the EC tests.
High removal percentages were obtained for all
metals analysed, with removals ranging from 86.92%
to 99.99% for total Cr, 87.05% to 97.63% for Cu,
79.27% to 96.94% for Mn and 87.11% to 99.99% for Ni.
The similarity between total Cr, Cu, Mn and Ni removal
percentages, observed in the tests 9, 10 and 11 (triplicate
central point), indicate that the pure error related to the
EC tests was low.
Since the maximum removal percentages were
obtained in different EC tests (no. 6, 8, 9, 10 and 11 for
total Cr; no. 2, 4, 6, 8, 9, 10 and 11 for Cu, Mn and Ni),
pH = 7.00, t = 22.5 min and DC = 17.5 mA/cm2 was con-
sidered as the ideal experimental condition (which cor-
responds to tests 9, 10 and 11). This experimental
condition operates at neutral pH and requires a lower

Figure 1. Removal percentages obtained after EC tests.


Figure 2. Pareto charts for (a) total Cr; (b) Cu; (c) Mn; (d) Ni.
volume of chemicals to pH adjustment. In addition, as
the reaction time (t) and current density (DC) applied
to tests 9, 10 and 11 are intermediate, it is possible to
reduce costs related to electricity consumption.
Statistical analysis on total Cr, Cu, Mn and Ni
removal percentages
The statistical analysis of Cr, Cu, Mn and Ni removal per-
centages was performed using Pareto charts, presented
in Figure 2 (considering a 95% confidence level).
Pareto chart of Ni indicates that all the variables eval-
uated and pHxt, pHxDC, txDC interactions were signifi-
cant. pH was the variable that most affected Ni
removal. pHxt and pHxDC interactions showed a nega-
tive effect and txDC interaction had a positive effect,
indicating that the highest percentages of Ni removal
were obtained at high pH values and at lower t and
DC. Pareto charts of Cu and Mn indicate that only pH
was significant in the removal of these metals, with
high removal percentages obtained when initial pH
ENVIRONMENTAL TECHNOLOGY 5
values were increased. For total Cr removal, none of
the variables evaluated was significant.
The results obtained were similar to those observed
by Al Aji et al. [41], Bhagawan et al. [42] and Xu et al.
[15]. Al Aji et al. [41] evaluated the efficiency of the EC
process in heavy metals removal, using iron electrodes.
The authors noted that removal efficiencies increase
generally at high pH values, because the majority of
iron complexes (coagulants) are formed at these pH
values. Percentages of Mn removal of approximately
8% were obtained at pH 3.00, 22% at pH 5.68 and
above 75% at pH 8.95 ([Mn]initial = 150 mg/L; DC = 25
mA/cm2; t = 45 min). Bhagawan et al. [42] evaluated
the treatment of a metal plating wastewater through
EC, for Cr, Cu, Pb, Ni and Zn removal. The authors
observed that metal removal efficiency increased with
the increase in pH, with maximum removal percentages
of Ni (96.4%) and Cu (97.5%) obtained at pH 8 (t = 30
min; applied voltage = 8 V). Xu et al. [15] identified that
high pH values facilitates Mn (II) removal. When the
6 B. M. FAVERO ET AL.
initial pH increased from 4 to 7, Mn (II) concentration
decreased from 203.3 to 166.5 mg/L after 60 min of
the EC treatment.
Influence of control variables on Cr, Cu, Mn and Ni
removal efficiencies
The discussions presented in this topic are based on the
results obtained after the EC tests (shown in Figure 1),
carried out at pH 3 and 11; t = 15 and 30 min; DC = 10
and 25 mA/cm2. Results related to the ideal experimen-
tal condition (tests 9–11 – triplicate of the central point)
were not included in this discussion.
Effect of initial pH. In the analysis of the initial pH
influence were considered each pair of EC tests, carried
out with pH variation (3 and 11) and keeping the par-
ameters t (15 or 30 min) and DC (10 or 25 mA/cm2) con-
stant. Figure 3 shows the comparisons between the
removal percentages obtained for Cr, Cu, Mn and Ni in
each pair of EC tests.
The comparison between tests 1 and 2 (a), 3 and 4 (b),
5 and 6 (c), 7 and 8 (d) indicates that the highest removal
percentages of Cr, Cu, Mn and Ni were obtained at pH 11
(tests 2, 4, 6 and 8). pH is one of the important factors in
affecting the performance of electrochemical process
[43], and is related to the coagulant in solution, that
Figure 3. Comparison between EC tests performed under the same experimental conditions (t and DC) and with pH variation (3 and
11). (a) Tests 1 and 2 (t = 15 min; DC = 10 mA/cm2); (b) 3 and 4 (t = 30 min; DC = 10 mA/cm2); (c) 5 and 6 (t = 15 min; DC = 25 mA/cm2);
(d) 7 and 8 (t = 30 min; DC = 25 mA/cm2).
presents different species in equilibrium depending on
the pH [44]. When EC is performed with iron electrodes,
monomeric species, Fe(OH)3 and polymeric hydroxy
complexes can be formed [45], which act to a greater
or lesser extent in the removal of metal ions.
According to predominance zone diagram for Fe2
+
and Fe3+, proposed by Garcia-Segura et al. [44], Fe
(OH)2 precipitates at pH > 5.5 and is in equilibrium
with Fe2+(up to pH 9.5) e Fe(OH)+(pH 9.5–11.4), while
Fe(OH)3 coagulates since pH > 1.0 and is in equilibrium
with Fe(OH)2+(pH 2.0–3.8), Fe(OH)+2 (pH 3.8–6.2) and Fe
(OH)−4 (from pH 9.6). Fe(OH)3 is the unique species
present in solution in the range of pH between 6.2 and
9.6 [44]. At pH 11 (where the highest removal rates of
Cr, Cu, Mn and Ni occurred), Fe(OH)2, Fe(OH)+, Fe(OH)3
and Fe(OH)− 4 are present. This suggests that metals
removal occurred mainly by the action of the coagulants
Fe(OH)2 and Fe(OH)3, since species such as Fe(OH)− 4
present poor coagulative activity [44].
During the EC tests, changes in the solution pH were
observed. Figure 4 shows pH variations of the effluent
samples, observed before and after the EC tests.
Moderate increases in the initial pH values of the
samples were observed in all EC tests. In acidic initial
pH (tests 1, 3, 5 and 7) the most significant variation
was observed in test 7 (performed with 25 mA/cm2 for

Figure 4. Initial and final pH values measured before and after EC tests.
30 min), where the pH increased from 3 to 4.55 at the
end of treatment. In basic pH (tests 2, 4, 6 and 8), the
sample related to test 8 (25 mA/cm2; 30 min) showed
the greatest variation between initial and final pH
(from pH 11 to 12.02). In neutral pH (tests 9–11), the
average of the final pH values was 7.59 ± 0.07.
According to Mansoorian et al. [46], changes in the pH
value during the EC process are influenced by the type/
material of the electrode used and the initial pH of the
effluent. In this sense, the use of iron electrodes
implies an increase (to a greater or lesser degree) of
the initial acid pH values (pH <7), due to the evolution
of H2 gas and generation of OH− ions at the cathodes
[47,48]. At initial alkaline pH (pH> 8), the final pH does
not change markedly because the generated OH− ions
at the cathodes are consumed by the generated Fe3+
ions at the anode, forming Fe(OH)3 flocs [47]. In
neutral medium there are small increases in the initial
pH, also caused by the production of OH− ions at the
cathode and by the buffering capacity of that pH [49].
The most significant pH elevations obtained at the
highest DC value indicate that probably the generation
of OH− ions in the cathodes was higher than the concen-
tration consumed by the iron ions to form coagulating
agents, as pointed out in the studies by Mollah et al.
[50] and Vepsäläinen et al. [51]. Moderate elevations of
the initial pH with increasing values of DC were also
identified in the study by Lekhlif et al. [52].
Effect of current density and reaction time. Current
density is an important EC parameter that directly deter-
mines both coagulant dosage and bubble generation
rates [53]. This parameter is directly related to the reac-
tion time, since the duration of electrolysis affects the
amount of released iron in a system and determines
the amount of produced Fe3+ [54]. In the analysis of
the current density influence were considered each
ENVIRONMENTAL TECHNOLOGY 7
pair of EC tests performed with DC variation (10 and
25 mA/cm2) and keeping the pH (3 or 11) and t (15 or
30 min) constant, as Figure 5.
Comparing the results obtained for each pair of EC
tests (Figure 5), removal percentages of Cr, Cu, Mn and
Ni are very similar at 10 and 25 mA/cm2. Cr maximum
removal was obtained in tests 6 and 8 (performed at
10 mA/cm2). For Cu, Mn and Ni, maximum removals
were obtained in both evaluated DCs (tests 2, 4, 6, 8).
The effect of reaction time was analysed based on
each pair of EC tests, carried out with variation of t (15
and 30 min) and maintaining the parameters pH (3 or
11) and DC (10 or 25 mA/cm2) constant. Figure 6
shows these results.
The results obtained for the pairs of EC tests 1 and 3 (a);
5 and 7 (c) (Figure 6) shows that, the longer the reaction
time, the greater the removal percentage achieved (with
the exception of Mn, which showed a removal of 79.27%
after 30 min of EC versus 83.48% after 15 min of treatment
(in tests 1 and 3, performed at pH 3 and 10 mA/cm2)).
However, in tests 2 and 4 (b); 6 and 7 (d) (performed at
pH 11, 10 and 25 mA/cm2, respectively), identical
removal percentages were observed after 15 and 30
min of treatment, indicating that the increase in t
values was not significant for Cr, Cu, Mn and Ni removal.
According to Al-Qodah and Al-Shannag [19], in the EC
process, the concentration of the produced coagulant
from the anode increases with time, favouring metals
removal. The same occurs with DC increase, that
implies a greater iron release from the anodes, providing
a greater production of coagulants in the aqueous
medium and, consequently, a superior removal of con-
taminants. However, the system can reach the
maximum removal point at lower t and DC values, so
that at higher values than the ideal t and DC, the
removal efficiency of pollutants remains constant (as
was observed in the present study), because the
8 B. M. FAVERO ET AL.

Figure 5. Comparison between EC tests carried out under the same experimental conditions (pH and t) and with DC variation (10 and 25
mA/cm2). (a) Tests 1 and 5 (pH 3; t = 15 min); (b) 2 and 6 (pH 11; t = 15 min); (c) 3 and 7 (pH 3; t = 30 min); (d) 4 and 8 (pH 11; t = 30 min).

Figure 6. Comparison between EC tests performed under the same experimental conditions (pH and DC) and with variation of t (15
and 30 min). (a) Tests 1 and 3 (pH 3; DC = 10 mA/cm2); (b) 2 and 4 (pH 11; DC = 10 mA/cm2); (c) 5 and 7 (pH 3; DC = 25 mA/cm2); (d) 6
and 8 (pH 11; DC = 25 mA/cm2).

Figure 7. Initial and final conductivity values measured before and after EC tests.
medium contains sufficient quantity of coagulants flocs
available for pollutant removal. [19]
Considerations about the conductivity evolution
during EC tests
The evolution of the initial and final conductivity during
the EC tests is shown in Figure 7.
Reductions between the initial and final conductivity
values were observed in tests 1, 3, 5, 7, conducted at pH
3 and performed with different DC and t values (10 and
25 mA/cm2; 15 and 30 min, respectively) and in exper-
iments 9, 10, 11, related to the triplicate central point
(pH 7; 17.5 mA/cm2; 22.5 min). In the tests carried out
in acid pH, the greatest reduction in the conductivity
value occurred in test 1 (from 12.48 to 10.00 mS/cm),
while in the tests related to the triplicate central point,
an average variation of 12.33 ± 0.17–11.43 ± 0.11 mS/
cm was observed. In contrast, tests 2, 4, 6 and 8,
carried out at pH 11 and performed at different DC
and t values (10 and 25 mA/cm2; 15 and 30 min, respect-
ively), presented elevations between initial and final
conductivity values. Among these tests, the most pro-
nounced increase occurred after the execution of test
8 (from 11.67 to 17.03 mS/cm).
Conductivity is a parameter directly proportional to
the presence of ions in solution. Therefore, declines
between the initial and final conductivity values
observed in acidic and neutral pH can be attributed to
the decrease in the amount of ions in the aqueous
medium. Regarding the increase in conductivity at
basic pH, the effect of adding NaOH to the aqueous
medium (for initial pH adjustment) should be con-
sidered, since NaOH added to the effluent supplies
ions to the solution, through its dissociation. Adjusting
the original effluent pH (pH 2.70) to alkaline pH (pH
11) demands a higher volume of NaOH when compared
ENVIRONMENTAL TECHNOLOGY 9
to that needed to adjust the acidic (pH 3) and neutral
(pH 7) pH, which justifies the greater presence of ions
in solution, and consequently, in a high conductivity,
observed in alkaline pH.
The increase in final conductivity observed in test 8
(pH 11; 25 mA/cm2; 30 min) may be also related to the
increase in iron release rate from the anodes, provided
by the high DC applied to the system. Similar results
to those obtained in this study were verified by Zarei
et al. [55] and Afsharnia and Saeidi [56].
Characterization of treated effluent
Table 2 shows the results obtained after the characteriz-
ation of treated effluent in the ideal EC condition (pH
7.00; t = 22.5 min; DC = 17.5 mA/cm2). This results were
compared to the maximum limits established in Brazilian
legislation (CONAMA Resolution 430/2011) [57], for
industrial effluents discharge into water bodies.
Results indicate that EC was efficient in removing
most of the metals and/or chemical elements originally
contained in effluent. In the optimal treatment con-
dition, it was possible to meet the maximum concen-
trations for the discharge of effluents into the aquatic
environment (established in Brazilian legislation) for
most of the elements evaluated, with the exception of
As, Pb, Mn and Se. An alternative for the removal of
this chemical elements is the combination of the EC
process with chemical precipitation, since Pb and Mn
precipitate in the hydroxide form at high pH values
[58–60]. Removal of residual As and Se can also be per-
formed through chemical precipitation, with sulphides
addition. Considering that this chemical elements are
present in reduced concentrations in the treated
effluent (<0.20 to <4.00 mg/L), the complementary treat-
ment cost would be low, since it would require a lower
volume of chemicals for pH adjustment.
10 B. M. FAVERO ET AL.

Table 2. Characterization of treated effluent and maximum some diffraction peaks of reduced intensity. The low crys-
limits established in CONAMA Resolution 430/11. tallinity seems to be a specific characteristic of galvanic
Maximum sludge from real or synthetic effluents, being described
concentration
Raw Treated effluent CONAMA Resolution in other studies, such as those by Chen et al. [62], Li
Parameter effluent (Tests 9, 10 and 11) 430/2011 et al. [63] and Xia et al. [64]. Despite this aspect, it was
Al (mg/L) 16.29 1.37 ± 0.67 n.e. possible to identify characteristic diffraction peaks of
As (mg/L) <2.00 <2.00 ± 0.00 0.50
Ba (mg/L) 4.48 0.87 ± 0.25 5.00 Fe2O3 (2θ = 11.35°, 14.90°, 18.20°, 23.85°, 26.03°, 34.11°,
Cd (mg/L) 0.47 <0.20 ± 0.00 0.20 53.96°, 62.80° and 71.40°), Fe3O4 (2θ = 30.40°, 36.06°,
Ca (mg/L) 336.77 265.31 ± 106.77 n.e.
Pb (mg/L) 2.15 <2.00 ± 0.00 0.50 37.97°, 44.06°, 54.47° and 63.92°) and Fe2(CrO4)3.3H2O)
Co (mg/L) 1.51 <0.40 ± 0.00 n.e. (2θ = 12.32°, 28.11° and 58.00°). These compounds had
Cu (mg/L) 25.29 <0.60 ± 0.00 1.00 tetragonal, cubic and monoclinic structures, respectively,
Conductivity 12.54 11.43 ± 0.11 n.e.
(mS/cm) and were indexed to the crystallographic information
Cr (mg/L) 4989.42 <0.40 ± 0.00 n.e. cards COD 1528612, 9002323 and 2106426 [40].
S (mg/L) 177.92 139.58 ± 63.14 n.e.
Fe (mg/L) 3085.79 <4.00 ± 0.00 15.00 The presence of iron compounds in the sludge
P (mg/L) 6.33 2.51 ± 3.48 n.e. sample is justified by its high initial concentration in
Mg (mg/L) 283.48 139.79 ± 2.36 n.e.
Mn (mg/L) 130.65 <4.00 ± 0.00 1.00 raw effluent (3085.79 mg/L), by the removal percentage
Ni (mg/L) 3560.09 0.45 ± 0.09 2.00 obtained under ideal treatment conditions (99.87%) and
pH 2.70 7.59 ± 0.07 5.00–9.00
K (mg/L) 4.95 26.06 ± 3.37 n.e.
due to the iron released from the anodes during EC.
Se (mg/L) <4.00 <4.00 ± 0.00 0.30 Moreover, Fe2O3 and Fe3O4 compounds have often
Na (mg/L) 448.88 1934.16 ± 66.07 n.e. been identified in diffractograms related to sludge
V (mg/L) <0.20 <0.20 ± 0.00 n.e.
Zn (mg/L) 14.21 < 2.00 ± 0.00 5.00 obtained after treating effluents from different sources
n.e., Not specified. through EC with iron electrodes, as in the studies by
Aytac and Un [65], Hafez et al. [66] and Fu et al. [67].
Characterization of the sludge generated From the reactions of Fe2O3 and Fe3O4 formation
In the ideal treatment condition (tests 9, 10 and 11) an (Equations (10) and (11)) suggested by Moreno-Casillas
average mass of 12.67 ± 0.35 g of galvanic sludge was [68] and Aytac and Un [65], it can be inferred that Fe
obtained. The precipitate was subsequently analysed (OH)3 and Fe(OH)2 acted as coagulants in the removal
through XRD and SEM techniques, according to of metals contained in the galvanic effluent evaluated
Figures 8 and 9. in this study.
SEM images indicate that the surface of the galvanic 2Fe(OH)3
Fe2 O3 + 3H2 O (10)
sludge obtained in the ideal treatment condition has
varying sizes of flak-shaped aggregates. The sludge par- 2Fe(OH)3 + Fe(OH)2
Fe3 O4 + 4H2 O (11)
ticles were irregular indicating its amorphous nature
[35]. A similar sludge aspect was observed in the study
performed by Hamdan and El-Naas [61], who carried Production of inorganic pigments
out the treatment of brackish groundwater through EC 8.27 g of brown inorganic pigment were obtained from
with iron electrodes. 10 g of the mixture of Al2O3, TiO2 and galvanic sludge
The galvanic sludge generated under EC ideal con- (with loss of 17.25% of the material after calcination).
dition showed low crystallinity, with the presence of Preliminary tests carried out with the mixture of

Figure 8. SEM images of the galvanic sludge generated in tests 9, 10 and 11. (a) 245X; (b) 500X; (c) 2000X magnification.
 ENVIRONMENTAL TECHNOLOGY 11

Figure 9. Diffractogram obtained for the galvanic sludge sample generated in the ideal treatment condition.

Figure 10. SEM images of the inorganic pigment (10% galvanic sludge + Al2O3, TiO2). (a) 500X; (b) 2000X; (c) 6500X magnification.

pigment and transparent glaze indicated good adhesion The inorganic pigment produced from the mixture of
of the pigment to a tile, remaining intact even after suc- oxides and 10% of galvanic sludge presented aggregates
cessive washes. Figure 10 shows the micrographs with irregular spherical morphology (Figure 10a) and par-
obtained for the inorganic pigment produced. ticles with grain size distribution below 10 µm (Figure 10c).

Figure 11. Diffractogram obtained for the inorganic pigment produced from the mixture of Al2O3, TiO2 and 10% of galvanic sludge.
12 B. M. FAVERO ET AL.
The morphology of the pigment containing 10% galvanic
sludge is different from that found in pure-based pig-
ments, which have a spherical structure. According to
Milanez et al. [69], this occurs due to the micronization
process to which the industrial pigment is submitted.
The pigment containing 10% of galvanic sludge was
grinded after calcination only with mortar and pistil,
which may have contributed to the irregular morphology
observed in the micrographs. Figure 11 shows the diffrac-
togram obtained for the inorganic pigment.
The inorganic pigment produced with 10% of galva-
nic sludge presented crystalline phases associated with
Al1.82Cr0.18O3/corundum (2θ = 25.62°, 35.21°, 37.85°,
43.42°, 52.64°, 57.59°, 61.35°, 66.64° and 68.31°), Ca0.999-
(Ti0.805Fe0.201)O2.899 (2θ = 23.30°, 33.17°, 40.68°, 47.59°,
59.04° and 69.57°), Fe2.18O4Ti0.42/titanomaghemite (2θ
= 35.82° and 63.19°) and TiO2 (2θ = 27.48° and 35.98°).
These compounds showed, respectively, trigonal,
orthorhombic, cubic and tetragonal crystalline structure
and were indexed to the crystallographic information
cards COD 9008094, 1525942, 9001114, 4102355 [40].
The identification of two low intensity peaks related to
TiO2, indicates that the oxide did not fully react with
Al2O3 and other components of the galvanic sludge
during pigment production, possibly due to the excess
addition of TiO2 to the reaction medium.
Conclusion
The present study evaluated the efficiency of EC process in
the treatment of a galvanic effluent, aiming total Cr, Cu, Mn,
Ni removal and the reuse of the sludge generated for inor-
ganic pigment production. The influence of pH, t and DC in
EC treatment was evaluated through factorial design 23
with triplicate central point. Experimental results showed
that pH = 7,00; t = 22.5 min; and DC = 17.5 mA/cm2 was
the ideal treatment condition. In this experimental con-
dition, removals of 96.94%, 97.63%, 99.99% and 99.99%
were obtained for Mn, Cu, total Cr and Ni, respectively,
allowing to meet the limits provided for in Brazilian legis-
lation for industrial effluents discharge into the aquatic
environment (CONAMA Resolution 430/2011).
Inorganic pigment production (with Al2O3, TiO2 and
10% of galvanic sludge) proved to be technically feas-
ible, obtaining at the end of the process 8.27 g of
brown inorganic pigment, composed mainly of Al1.82-
Cr0.18O3, Ca0.999(Ti0.805Fe0.201)O2.899 and Fe2.18O4Ti0.42.
The results obtained in this study show that EC is a
promising technique for the treatment of galvanic
effluents. The sludge produced during treatment is rich
in heavy metals and therefore has the potential to be
reused in inorganic pigment production, reducing the
environmental impact related to electroplating process.
Disclosure statement
No potential conflict of interest was reported by the author(s).
Funding
This study was financed in part by the Coordenação de Aper-
feiçoamento de Pessoal de Nível Superior - Brazil (CAPES) -
Finance Code 001.
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