Simultaneous Removal of Cd2+ and Zn2+ Ions From Aqueous Solution Using Upflow Al-Electrocoagulation

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1297 © 2019 The Authors Water Science & Technology | 79.7 | 2019
Simultaneous removal of Cd2þ and Zn2þ from aqueous

solution using an upflow Al-electrocoagulation reactor:
optimization by response surface methodology
Vianey Ariadna Burboa-Charis, Eddy Jonatan Moreno-Román,
Juan Antonio Vidales Contreras and Celestino García-Gómez
ABSTRACT
The presence of heavy metals in the environment has increased, and cadmium (Cd) and zinc (Zn) are Vianey Ariadna Burboa-Charis
Departamento de Biotecnologia y Ciencias
considered to be among the most dangerous. An upflow Al-electrocoagulation reactor was used to Alimentarias,
Instituto Tecnologico de Sonora (ITSON),
remove Cd2þ and Zn2þ ions from aqueous media. The system consisted of perforated aluminum 5 de Febrero 818 Sur C.P. 85000 Cuidad Obregon,
Sonora,
circular electrodes for fluid distribution with elimination of external agitation. The effect of different
Mexico
parameters, i.e. current intensity, electrolysis time, concentration of Cd2þ and Zn2þ ions and
Eddy Jonatan Moreno-Román
electrolytic support dose were optimized by response surface methodology. The results indicated that Facultad de Ingeniería Civil,
Universidad Autónoma de Nuevo León, Cd.
increasing the current intensity and the electrolysis time had a positive effect on the elimination Universitaria,
Av. Universidad S/N, San Nicolás de los Garza
efficiency of the pollutant ions. Likewise, increasing the dose of electrolytic support and decreasing the
66455, Nuevo León,
concentration of the pollutants improved the efficiency of the system. The optimal results were: México
current intensity of 0.4 A, electrolysis time of 40 min, ion concentration of 44.6 mg·L1 and electrolytic Juan Antonio Vidales Contreras
1 Celestino García-Gómez (corresponding
support dose of 0.56 mg·L , with the maximum elimination percentages of 96 ± 3.8% and 96 ± 2.7% author)
Facultad de Agronomía,
for Cd2þ and Zn2þ, respectively. This study showed that the electrocoagulation process in an upflow
Universidad Autónoma de Nuevo León,
electrocoagulation reactor could be successfully applied to remove pollutants from water. Francisco Villa S/N, C. P. 66050 General Escobedo,
Nuevo León,
Key words | central composite design, electrocoagulation, heavy metals, removal, response surface México
E-mail: celestino.garciagm@uanl.edu.mx
methodology
INTRODUCTION
The contamination of water by heavy metals has become metal and its bioavailability determines the physiological
a serious environmental problem. Heavy metals are dis- and toxic effects on living organisms (Olaniran et al. ).
charged from a variety of sources, and can easily Cadmium (Cd) can be found in high doses in seafood, veg-
be separated into ions when they are dissolved in water etables, cereals, products of animal origin and even in
(Ecer et al. ). Heavy metals are widely found in soil chocolate; it produces toxic effects on various tissues such
and aqueous systems, either naturally or as a result of anthro- as the kidneys, liver, testicles, lungs and bones (Vasudevan
pogenic human activities via agricultural, industrial and & Lakshmi ). Zinc (Zn) is an essential element due to
mining operations (Xu et al. ). Heavy metal pollution is its participation in a variety of biological processes but an
currently a major environmental problem because metal excess of Zn produces effects including depression, gastroin-
ions persist in the environment due to their non-degradable testinal irritation, impotence, kidney and liver failure,
nature, and the toxicity and bioaccumulation tendency lethargy and prostate cancer (Gumpu et al. ). All the nega-
of heavy metals is a serious threat to the health of living tive effects described have generated scientific interest in the
organisms (Ayangbenro & Babalola ). Speciation of a efficient removal of heavy metals from water.
The main strategies used to address the problem of
This is an Open Access article distributed under the terms of the Creative eliminating metal ions from water are: chemical precipi-
Commons Attribution Licence (CC BY-NC-ND 4.0), which permits copying
tation, solvent extraction, reverse osmosis processes,
and redistribution for non-commercial purposes with no derivatives,
provided the original work is properly cited (http://creativecommons.org/
adsorbents, and electrochemical treatments (Ecer et al.
licenses/by-nc-nd/4.0/). ).
doi: 10.2166/wst.2019.123
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1298 V. A. Burboa-Charis et al. | Removal of Cd2þ and Zn2þ using an upflow electrochemical reactor Water Science & Technology | 79.7 | 2019
In recent years, electrocoagulation has been used distilled water. Ions of Cd2þ and Zn2þ were used as model
successfully to treat a variety of industrial wastewaters pollutants. Synthetic solutions were prepared with zinc
(Xu et al. ). Four main processes occur during electro- sulfate heptahydrate (ZnSO4·7H2O) and cadmium sulfate
coagulation: electrolyte reactions on the surface of the hydrate (CdSO4·8/3H2O) at pH ¼ 7. Sodium sulfate
electrodes, formation of coagulants in the aqueous phase, (Na2SO4) (purity 99%) was used as an electrolyte support
adsorption of soluble or colloidal pollutants in the coagu- at a fixed concentration of 400 mg·L1 to increase the
lants and elimination by sedimentation (Al-Shannag et al. conductivity of the aqueous medium. At the end of
). The main electrochemical reactions occurring in the each experiment, the treated effluent was subjected to sedi-
anode, cathode, and solution for aluminum electrodes are mentation for 30 min. Then, the supernatant was filtered
as follows (Mollah et al. ): Al(s) ↔ Alþ3
(aq) þ 3e in the under vacuum using a 0.45 μm cellulose membrane filter

anode, 2H2 O þ 2e ↔ H2(g) þ 2OH(aq) in cathode, and for (Millipore, EZ-Pak) and analyzed by atomic absorption
the overall reaction 2Al(aq) þ 6H2 O ↔ 2Al(OH)3 (s) þ 3H2 (g) . spectroscopy (AA Series, ThermoFisher Scientific with
In the electrocoagulation process, factors such as cur- FS95 furnace autosample).
rent intensity and electrolysis time influence the efficiency
of the process, which can be increased by optimizing these Experimental setup and procedure
factors (Gatsios et al. ).
The design of reactors on an industrial scale is based A cylindrical upflow reactor was used in this study. The
on empirical criteria due to the lack of available models experimental system was made of polycarbonate with
that include the main factors that allow their optimization dimensions of 24.5 cm (height) and 7.2 cm (internal diam-
(Gatsios et al. ). These models should consider factors eter). In the interior was a set of six electrodes in a
that influence the physicochemical, electrochemical and circular aluminum plate with a diameter of 6.5 cm and a
hydraulic stages of the process, as well as their interactions thickness of 5 mm, with an active surface area of 66.4 cm2
(Tak et al. ). However, the mechanisms of electrocoagula- per electrode. Each electrode was drilled to obtain 10
tion have not yet been clearly understood, and in most of the holes of 5 mm in diameter. There was an inter-electrode dis-
existing work only the efficiencies for test conditions have tance of 2 cm to ensure good mixing and aeration efficiency
been established and the factors that influence the effective of the fluid. The solution (1 L) was pumped upwards at
removal of ionic species of metallic ions from water not 150 ml L1 through a peristaltic pump connected at the
been analyzed (Brillas & Martínez-Huitle ). bottom of the column. All the experimental runs were car-
The main motivation of this study is to evaluate the ried out at room temperature (23 ± 1 C) and atmospheric
removal efficiency without external stirring for a good pressure. The electrodes were connected to a DC power
distribution of the fluid by a new configuration of electrocoa- supply with variable voltage (Bk Precision, 0–32 V, 0–3 A)
gulation systems. Several studies in the literature have as a source of electrical energy, and the amperage was con-
reported the removal of metal ions using electrocoagulation tinuously controlled. To remove impurities from the surface
systems, but no studies were found for the simultaneous after each run of electrocoagulation, the electrodes were
removal of cadmium and zinc in upflow reactors that elimin- sanded and immersed in diluted HCl (5% v/v) solution
ate any external stirring. Therefore, the overall objective of then washed with distilled water. The removal efficiency of
this study was the optimization of different operating par- Cd2þ and Zn2 concentration was calculated according to
ameters (current intensity, electrolysis time, concentration of Equation (1):
pollutant ions and electrolytic support dose) in an upflow
reactor by response surface methodology (RSM) for the sim- C0 C
ultaneous removal of Cd2þ and Zn2þ from aqueous solution. removal (%) ¼ (1)
C0
where C0 and C were the initial and residual Cd2þ and Zn2þ
MATERIALS AND METHODS concentrations (mg·L1), respectively.
Synthetic solutions of Cd2þ and Zn2þ

Experimental design and optimization
The synthetic solutions used for the electrocoagulation tests An experimental design using RSM, especially central com-
were prepared from chemical reagents of analytical grade in posite design (CCD), was used to study the interaction of

by guest
independent variables and optimize the electrocoagulation where b0 , bi , bii and bij are respectively the regression poly-
system. CCD is a mathematical and statistical strategy that nomial coefficients for: linear, quadratic and interaction,
uses experimental quantitative data to generate a regression while Xi and Xj are the coded independent variables.
model among the factors (independent variables) and the
response variables (Asfaram et al. ). A CCD produces
a polynomial surface and reduces the number of experimen- RESULTS
tal runs N, according to Equation (2):
Design of experiment by CCD
N ¼ 2 þ 2k þ n0
k
(2)
A four-factor CCD with five levels was applied to evaluate
where k is the number of factors, 2k represents factorial and optimize the effects of the variables involved in the
runs, 2k axial runs and n0 central points or replicas. electrocoagulation system in the response variables, i.e.
Initially, some random runs were performed to the removal efficiency of Cd2þ (Y1 ) and Zn2þ (Y2 ). A total
determine the operating parameters range in the electroche- of 26 experiments in a random order were carried out
mical treatment. The performance of the electrocoagulation with six repetitions of the central values in the design.
system was evaluated and optimized with a CCD for four Table 2 shows all the experiments, the experimental
factors, i.e. current intensity (X1) of 0.1–0.5 A, electrolysis values, and the experimental responses of Cd2þ and Zn2þ
time (X2) of 10–50 min, concentration of Cd2þ and Zn2þ removal together with predicted values.
ions (X3) of 20–60 mg·L1 and electrolytic support dose
(X4) of 0.25–1.25 mg·L1, with five levels in the design Development of the regression model and statistical
(α, low, central, high and þ α) which are shown in Table 1. analysis
The performance of the electrocoagulation system was
determined by analyzing the removal efficiency of the In order to determine the best model adjusted to the exper-
Cd2þ and Zn2þ ions. The statistical software Design Expert imental data, the Design Expert software was used to
(7 trial version, Stat-Ease, Inc.) was used to generate the select the correct regression model among several types
regression analysis and graphs from the experimental data of proposed models, such as linear, 2FI, quadratic and
generated. An analysis of variance (ANOVA) was performed cubic. The results of a sequential model sum of squares
to determine the significant effects of the system variables test, lack-of-fit and model summary statistics are presented
and the adjustment of the data. The experimental response in Tables 3 and 4 for the response variables Y1 and Y2 ,
according to the CCD matrix was represented by a second- respectively, which are the functions of the independent
order polynomial model, according to Equation (3): variables current intensity (X1), electrolysis time (X2),
concentration of Cd2þ and Zn2þ ions (X3) and electrolytic
X
k X
k XX
k support dose (X4).
Y ¼ b0 þ bi Xi þ bii X2i þ bij Xi Xj þ e (3) The appropriate model was selected according to high
i¼1 i¼1 j i¼2
values of standard deviation and a coefficient of determi-
nation for each response. As shown in Table 3, for the
removal of Cd2þ (Y1 ) the quadratic model (with the low
Table 1 | The factors and levels of the experimental design standard deviation of 11.57 and the high determination coef-
ficient of 0.9038) was selected, which would give predicted
Levels
values close to the actual values, with a residual minimum.
α Low Central High þα In addition, the cubic model was aliased, which means
Variables Factor (1.41) (1) (0) (1) (þ1.41)
that the model is inappropriate for studying the experimen-
Current intensity (A) X1 0.1 0.2 0.3 0.4 0.5 tal field. In the same statistical way, the removal of Zn2þ
Electrolysis time X2 10 20 30 40 50 (Y2 ) was analyzed and again a quadratic model was pro-
(min) posed (with the low standard deviation of 6.98 and the
Ions of Cd2þ and X3 20 30 40 50 60 high determination coefficient of 0.9001), as shown in
Zn2þ (mg·L1)
Table 4.
Electrolytic support X4 0.25 0.5 0.75 1 1.25 Besides that, an adequate precision of 12.361 and
(mg·L1)
12.017 for the removal of Cd2þ and Zn2þ, respectively,

by guest
Table 2 | Experimental design matrix and response based on the experimental runs and predicted values of Cd
2þ
and Zn2þ removal (%) proposed by CCD design
Y1 : Cd2þ removal (%) Y2 : Zn2þ removal (%)

X1 X2 X3 X4
1 1
Run (A) (min) (mg·L ) (mg·L ) Actual Predicted Actual Predicted
1 0.30 50 40 0.75 99.5966 100 99.6432 93.68

2 0.20 20 50 1.00 52.0423 50.53 48.6092 39.87
3 0.20 20 50 0.50 66.3776 62.19 11.5825 3.61
4 0.30 30 40 0.25 96.3676 98.67 46.8712 39.54
5 0.10 30 40 0.75 54.9063 67.47 21.2894 31.2
6 0.30 30 40 1.25 95.2867 96.55 79.0397 91.74
7 0.40 20 30 0.50 89.7686 96.53 44.5117 39.01
8 0.30 30 60 0.75 72.4019 75.51 28.5282 31.86
9 0.30 30 40 0.75 98.6479 98.17 54.3786 63.4
10 0.30 30 40 0.75 97.2118 98.17 49.8835 63.4
11 0.30 10 40 0.75 60.6533 63.15 18.7786 30.16
12 0.20 40 30 0.50 85.0584 79.73 26.4592 36.51
13 0.20 40 30 1.00 97.9443 99.59 97.8777 80.45
14 0.40 40 50 0.50 99.9876 100 99.9965 100
15 0.50 30 40 0.75 99.4486 90.47 95.7708 91.28
16 0.40 40 30 1.00 98.0582 100 97.7213 1000
17 0.20 20 30 0.50 79.0678 78.25 9.99061 11.17
18 0.40 20 50 0.50 87.7189 81.19 24.2253 32.53
19 0.20 40 50 0.50 99.3667 94.83 54.9406 49.19
20 0.30 30 40 0.75 99.584 98.17 73.2292 63.4
21 0.40 20 50 1.00 52.5657 59.21 44.9309 40.79
22 0.40 20 30 1.00 99.0085 98.67 99.2157 93.67
23 0.30 30 40 0.75 96.8333 98.17 72.7476 63.4
24 0.40 40 30 0.50 97.4454 94.05 96.0671 95.67
25 0.30 30 40 0.75 98.2448 98.17 69.9221 63.4
26 0.30 30 40 0.75 98.4785 98.17 60.2653 63.4
indicated that the quadratic models could indeed be used to terms of the model are statistically significant. When
explore the design space of the study, given that these values a P-value is greater than 0.1, the factors are not statisti-
were greater than 4. cally significant. In this study, X1, X2, were highly
Additionally, the adequacy of the model was verified significant, together with a significance on the part of
by an ANOVA analysis (Tables 5 and 6). ANOVA the factors X3, X4, X1X2, X1X4, X2X3, X2X4 and X21 for
showed that both quadratic models proposed according the removal of Cd2þ, while the remaining terms of the
to the experimental design, which were generated by model were not significant for this response. Table 6
an RSM using a CCD, can effectively satisfy the shows that a model F-value of 9.65 and the P-value of
modeling to predict the optimal conditions and to the model of less than 0.0001 indicate that the terms of
verify the interactive effect of independent variables in the model for the removal of Zn2þ were statistically
the electrocoagulation system for the removal of Cd2þ significant. The factor X2 was highly significant while
and Zn2þ. Table 5 shows the results for the removal the factors X1, X3, X2X3, X21, X22, X23 were significant.
of Cd2þ. An F-value for the model of 11.30 and a According to the ANOVA results, the quadratic
P-value for a model smaller than 0.0001 show that the regression models that were generated are shown in

by guest
Table 3 | Sequential model sum of squares, lack-of-fit tests and model summary statistics for Cd2þ removal (%)
Sequential model sum of squares
Source Sum of squares df Mean square F-value Prob > F Remark
Mean vs total linear 111,000 1 111,000

Linear vs mean 17,980.12 4 4,495.03 13.27 <0.0001
2FI vs linear 253.33 4 63.33 0.41 0.7954
Quadratic vs 2FI 5,921.81 6 986.97 7.37 0.0004 Suggested
Cubic vs quadratic 1,476.67 8 184.58 1.59 0.2779 Aliased
Residual 813.61 7 116.23
Total 137,400 30 4,581.57
Lack-of-fit tests
Linear 7,964.99 20 398.25 3.98 0.0658

2FI 1,789.84 10 178.98 1.79 0.2706
Quadratic 2,043.18 14 145.94 1.46 0.3580 Suggested
Cubic 313.17 2 156.59 1.56 0.2967 Aliased
Pure error 500.43 5 100.09
Model summary statistics
Predicted residual error

Source Std. dev. R2 Adj. R2 Pre. R2 sum of squares Remark
Linear 18.40 0.6799 0.6287 0.5099 12,961.23

2FI 12.36 0.9134 0.8326 0.5829 11,030.12
Quadratic 11.57 0.9038 0.8532 0.6712 8,694.39 Suggested
Cubic 10.78 0.9692 0.8725 0.7325 45,817.60 Aliased
Equations (4) and (5): The comparison between the experimental value and the
predicted value is shown in Table 2 and in a normal prob-
ability diagram in Figure 2(a) and 2(b). From Figure 1, the
Cd2þ removal (%), Y1 ¼ 63:4 þ 15:02X1 þ 15:88X2 values predicted by the model coincide with the experimental
10:05X3 þ 13:05X4 þ 7:83X1 X2 þ 0:27X1 X3 data, given that all the points are close to a diagonal line,
(4)
7:00X1 X4 þ 5:60X2 X3 9:68X2 X4 which confirms that the model is adequate because the
11:6X3 X4 0:54x21 0:37x22 2:86x23 þ 0:56x24 residuals for the prediction of each response are minimal.
In order to verify the suitability of the quadratic
Zn2þ removal (%), Y2 ¼ 98:17 þ 5:75X1 þ 9:39X2 regression model, the diagnostics section of the Design
6:09X3 0:53X4 0:99X1 X2 þ 0:18X1 X3 Expert software was analyzed. First, Figure 2(a1) and 2(b1)
(5) show the standardized residuals for the removal efficiency
2:58X1 X4 þ 7:79X2 X3 þ 1:85X2 X4 6:03X3 X4
of Cd2þ and Zn2þ (%) respectively, and in accordance with
4:80x21 4:06x22 2:62x23 0:14x24
the normal probability test, have proved that the residual dis-
tributions of the models are common. In addition to that, as
where X1, X2, X3, and X4, Y1 and Y2 are the current illustrated in Figure 2(a2) and 2(a3) and 2(b2) and 2(b3), the
intensity (A), the electrolysis time (min), the concen- residual graphs of the two models are randomly distributed
tration of pollutant ions of Cd2þ and Zn2þ (mg·L1), without any specific patterns and trends, indicating that the
electrolytic support dose (mg·L1) and the corresponding quadratic models generated are adequate and accurate to
removal efficiency of Cd2þ and Zn2þ (%), respectively. use in the prediction of Cd2þ and Zn2þ removal responses.

by guest
Table 4 | Sequential model sum of squares, lack-of-fit tests and model summary statistics for Zn2þ removal
Sequential model sum of squares
Mean vs total linear 2.36900 1 2.36900

Linear vs mean 3,805.56 4 951.39 6.77 0.0008
2FI vs linear 1,728.19 6 288.03 3.07 0.0285
Quadratic vs 2FI 1,053.84 4 263.46 5.41 0.0067 Suggested
Cubic vs quadratic 648.97 8 81.12 6.92 0.0097 Aliased
Residual 82.09 7 11.73
Total 2.44300 30 8,141.79
Lack-of-fit tests
Linear 3,508.06 20 175.40 174.24 <0.0001

2FI 1,779.87 14 127.13 126.29 <0.0001
Quadratic 726.03 10 72.60 72.12 <0.0001 Suggested
Cubic 77.06 2 38.53 38.27 0.0009 Aliased
Pure error 5.03 5 1.01
Model summary statistics
Predicted residual error

Source Std. dev. R2 Adj. R2 Pre. R2 sum of squares Remark
Linear 11.85 0.5200 0.4432 0.2852 5,231.40

2FI 9.69 0.7561 0.6278 0.3917 4,451.81
Quadratic 6.98 0.9001 0.8069 0.4276 4,189.18 Suggested
Cubic 3.42 0.9888 0.9535 0.5172 1,1103.61 Aliased
Effect of parameters for the maximum response removal generated a greater removal of polluting ions. This phenom-
of Cd2þ and Zn2þ enon can be related to the increase of the products
generated in anodic oxidation promoting the formation of
This section introduces the interactive effect of the selected aluminum metal hydroxides, together with the formation
variables and their effect on the responses, which can be of H2 bubbles in the cathode, helping with the process of
evaluated through a graphical representation of statistical separation or flotation (Moreira et al. ). The dissolved
optimization using RSM. As a result, the three-dimensional ions of the sacrificial anode are developed with increasing
response diagrams are presented in Figures 3 and 4 for current intensity according to Faraday’s law (Dolati et al.
the removal efficiency of Cd2þ and Zn2þ (%) respectively. ). Because enough power was provided through the sol-
Those response surfaces were created according to the quad- ution, the dissolved metal ions were hydrolyzed and metal
ratic regression models generated in Equations (4) and (5) hydroxide species were formed. Therefore, floc production
with two independent variables within the experimental grew by increasing the removal efficiency of polluting ions.
range of this investigation. The response surfaces of removal In addition, a large number of gas bubbles produced
efficiency of Cd2þ and Zn2þ (%) showed a clear peak, which around the cathode due to the high current intensity facili-
indicates that the optimum conditions fell within the limits tated the binding of polluting particles to the hydroxides
of the proposed design. Figures 3(a), 3(c) and 4(a), 4(c) coagulants, and thus improved the elimination efficiency
show the effect of current intensity with electrolysis time, of these ions.
concentration of Cd2þ and Zn2þ ions and electrolytic sup- Similarly, Figures 3(a) and 4(a) show that with an
port dose; as expected, an increase in current intensity increase in the electrolysis time, greater removal of polluting

by guest
Table 5 | ANOVA of the second-order polynomial equation for Cd2þ removal (%)
Source Sum of squares df Mean square F-value Prob > F Remarks
Model 24,155.27 14 1,725.38 11.30 <0.0001 Highly significant

X1 5,417.04 1 5,417.04 35.48 <0.0001 Highly significant
X3 2,421.96 1 2,421.96 15.86 0.0012 Significant
X4 4,090.07 1 4,090.07 26.79 0.0001 Significant
X1 X2 980.21 1 980.21 6.42 0.0229 Significant
3
X1 X3 1.13 1 1.13 7.426 × 10 0.9325
X1 X4 784.70 1 784.70 5.14 0.0386 Significant
X2 X3 501.44 1 501.44 3.28 0.0900 Significant
X2 X4 1,500.62 1 1,500.62 9.83 0.0068 Significant
X21 2,153.71 1 2,153.71 14.11 0.0019 Significant
X22 8.13 1 8.13 0.053 0.8206
X23 3.84 1 3.84 0.025 0.8761
X24 224.96 1 224.96 1.47 0.2436
Residual 8.66 1 8.66
Lack of fit 2,290.28 15 152.69
Pure error 1,789.84 10 178.98
Cor total 500.43 5
Table 6 | ANOVA of the second order polynomial equation for Zn2þ removal (%)
Source Sum of squares df Mean square F-value Prob > F Remarks
Model 6,587.59 14 470.54 9.65 <0.0001 Highly significant

X1 792.75 1 792.75 16.27 0.0011 Significant
X3 891.31 1 891.31 18.29 0.0007 Significant
X4 6.76 1 6.76 0.14 0.7147
X1 X2 15.59 1 15.59 0.32 0.5801
X1 X3 0.54 1 0.54 0.011 0.9177
X1 X4 106.34 1 106.34 2.18 0.1603
X2 X3 970.03 1 970.03 19.90 0.0005 Significant
X2 X4 54.57 1 54.57 1.12 0.3067
X21 581.12 1 581.12 11.92 0.0035 Significant
X22 632.28 1 632.28 12.97 0.0026 Significant
X23 453.09 1 453.09 9.30 0.0081 Significant
X24 187.82 1 187.82 3.85 0.0685
Residual 0.53 1 0.53
Lack of fit 731.06 15 48.74
Pure error 726.03 10 72.60
Cor total 5.03 5 1.01

by guest
Figure 1 | Predicted vs actual values for (a) Cd2þ removal and (b) Zn2þ removal.
Figure 2 | Diagnostics plots for (a) Cd2þ removal and (b) Zn2þ removal: normal probability test (a1 and b1), residuals versus the predicted values (a2 and b2) and residual versus run number
(a3 and b3).
ions is achieved because as the reaction time was extended, Cd2þ and Zn2þ ions. This is due to the generation of metal
aluminum was continuously dissolved from the anodes and hydroxides being constant for an applied current intensity
it generated a quantity of hydroxides in contact with the pol- with the different concentrations of polluting ions. There-
lutants, thus improving the efficiency of removal of these in fore, for a higher concentration of ions, the rate of
the system (Hooshmandfar et al. ). From Figures 3(b) removal is lower compared to a lower ion concentration.
and 4(b) it can be seen that the percentage of removal The conductivity of an electrolyte solution is a key factor
decreases with an increase in the concentration of the in an electrochemical system. The conductivity determines

by guest
Figure 3 | Three-dimensional response surfaces for Cd2þ removal: (a) intensity–time, (b) intensity–ions; (c) intensity–electrolytic support; (d) time–ions; (e) time–electrolytic support;
(f) ions–electrolytic support.
Figure 4 | Three-dimensional response surfaces for Zn2þ removal: (a) intensity–time, (b) intensity–ions; (c) intensity–electrolytic support; (d) time–ions; (e) time–electrolytic support;
(f) ions–electrolytic support.
the resistance of the cell, while the properties of the solvent electrodes (Attour et al. ). The effect of the electrolytic
and the electrolyte determine their interaction with the elec- support dose in the reduction of polluting ions is shown in
troactive species and therefore influence the reactions of the Figures 3(c) and 4(c), where it can be seen that the

by guest
electrolytic support doses increased the removal efficiency respectively. The results of the experiments were very simi-
of the polluting ions, due to an increase in the ionic strength lar to those predicted by the model, which indicates that
of the solution, which caused the movement of ions to the CCD could be used effectively to optimize the par-
increase between the electrodes (Thiam et al. ). The ameters of the electrocoagulation system.
effect of the electrolysis time is also reflected in Figures
3(d), 3(e) and 4(d), 4(e), where increasing the reaction Possible removal path of metal pollutants by the
time showed a greater removal of the polluting ions, while electrocoagulation system
a decrease in the concentration of ions promoted a greater
elimination of these, as shown in Figures 3(d) and 4(d). An The removal of metal ions by electrocoagulation is attributed
increase in the electrolytic support dose improved the to the combined effect of different removal mechanisms
conductivity of the aqueous medium and the removal of (a)–(b) (Hooshmandfar et al. ; Mishima et al. ;
pollutants as previously discussed; see Figures 3(e) and 4(e). Mlakar et al. ), which are shown in Equations (6)–(8).
(a) Adsorption by aluminum hydroxide flocs is the main
removal pathway of metals (M) under an electrocoagula-
Optimization of the electrocoagulation system
tion system, which might be attributed to the link/bridge
structure formed among aluminum colloidal particles.
The study of the new electrocoagulation system requires the
optimization of conditions in order to minimize energy
2þ
losses and consequently treatment cost losses. To optimize M(aq) þ Al(OH)3 (s) ! colloidal particle (6)
the electrocoagulation system, criteria were defined to
achieve the desired objective, selected by adjusting the
When multiple metals are present in water, these metal
weight or importance, which could alter the characteristics
ions not only compete for the hydroxide ions produced at
of an objective. The target fields for the variables have five
the cathode, but also compete for sorption sites at the
options: none, maximize, minimize, objective and within
aluminum hydroxide floc surface.
the range. The desired objectives for the removal of Cd2þ
and Zn2þ were established as maximize. The independent (b) Chemical precipitation as hydroxides occurs especially
factors studied in this work were established within the at high initial concentrations of metal pollutants.
range of designed levels (current intensity: 0.1–0.5 A, elec-
2þ
trolysis time: 10–50 min, concentration of Cd2þ and Zn2þ M(aq) þ 2OH(aq) ! M(OH)2 (s) (7)
ions: 20–60 mg·L1 and electrolytic support dose: 0.25–1.25
mg·L1), in both cases with a corresponding importance (c) Cathodic reduction to metallic forms occurs when a
of 3. The optimal conditions predicted for this model are deposition layer is formed on the cathode surface.
presented in Table 7. Experiments were performed in
triplicate and the average results together with the standard 2þ
M(aq) þ 2e ! Zn(s) (8)
deviation are given in Table 7. The removal efficiencies of
Cd2þ and Zn2þ obtained were 96 ± 3.8% and 96 ± 2.7%
Comparison of Cd2þ and Zn2þ removal using
Table 7 | Optimum conditions predicted and verification results electrocoagulation system (according to the literature)
Parameter Value
The performance of an electrocoagulation system depends
Current intensity (A) 0.4 on several factors, such as the current intensity, type of
Electrolysis time (min) 39.91 electrode, inter-electrode distance, initial pH, inlet concen-
Ions concentration (mg·L1) 44.61 tration and electrolysis time. In the literature, it has
Electrolytic support (mg·L1) 0.56 been shown that removal of heavy metals can be accom-
Cd2þ removal (%) predicted 100 plished at various initial concentration values varying
between 10 and 2,000 mg·L1 (Al-Shannag et al. ; Gher-
Cd2þ removal (%) observed 96.22 ± 3.83
naout et al. ; Xu et al. ; Chen et al. ; Ecer et al.
Zn2þ removal (%) predicted 100
). Current intensity is an important parameter in electro-
Zd2þ removal (%) observed 95.66 ± 2.69
coagulation performance. The range of the current intensity

by guest
Table 8 | Comparison of the results of this study with previous studies
Metals Operational parameters Results References
2þ 2þ 1
Cd , Cu Electrode: Fe, water type ¼ model, C0 ¼ 10 mg·L , t ¼ 45 min 88, 82.4 Ghernaout et al. ()
Cd2þ Electrode: Zn, water type ¼ model, C0 ¼ 20 mg·L1, t ¼ 30 min 96.9 Vasudevan & Lakshmi ()
2þ 2þ 2þ 2þ 1
Cu , Ni , Zn , Mn Electrode: Fe, water type ¼ model, C0 ¼ 250 mg·L , t ¼ 40 min 96, 96 96, 72.6 Al-Shannag et al. ()
Cd2þ, Zn2þ, Mn2þ Electrode: Fe, water type ¼ model, C0 ¼ 15, 92, 320 mg·L1, 99.5, 99.9, 55 Xu et al. ()
t ¼ 60 min
Zn2þ Electrode: Al, water type ¼ model, C0 ¼ 50–2,000 mg·L1, 25–99.9 Chen et al. ()
t ¼ 50 min
Cd2þ, Zn2þ Electrode: Al, water type ¼ model, C0 ¼ 20–60 mg·L1, t ¼ 40 min 96, 96 This study
values varies and depends on several factors, such as the other hand, as the concentration of Cd2þ and Zn2þ ions
type and amount of pollutants to be eliminated. Results in increased, there was a decrease in the elimination efficiency
the literature show that the values of the current intensity tendency. The ANOVA analysis revealed a high R2 value for
applied for the removal of heavy metal ions were 0.1–3 A the regression model equation, thus showing the degree of
(Al-Shannag et al. ; Ghernaout et al. ; Xu et al. agreement of the quadratic model with the experimental
; Chen et al. ; Ecer et al. ). Electrolysis or treat- data. This work contributes to the simultaneous removal of
ment time is another important operating parameter for the heavy metals and the interaction of the operational and
removal efficiency of the pollutants, as the metal hydroxide response variables. This electrocoagulation system could
production from the anode increases with time. The selec- therefore be used effectively for the elimination of pollutants
tion of variables is an important factor for the removal of in drinking water, industrial effluents and sewage water.
the pollutants, and there are few studies that investigate
the removal of two or more metals simultaneously and the
interactions among the variables. Results of previous studies
ACKNOWLEDGEMENTS
for the removal of heavy metals using electrocoagulation are
shown in Table 8. The results show that electrocoagulation
Sincere thanks are extended to the National Council of
system is efficient at removing heavy metals from water.
Science and Technology (CONACYT) for the support pro-
vided in the form of postdoctoral fellowship no. 290941 to
Celestino García-Gómez.
CONCLUSIONS
In the present investigation an effective application was

CONFLICT OF INTERESTS
demonstrated for the removal of metals as Cd2þ and Zn2þ
under statistical optimization, using an upflow Al-electro-
The authors have no conflict of interests.
coagulation reactor, with the purpose of suggesting new
configurations in the design of electrocoagulation reactors
to eliminate a system of agitation and improve fluid distri-
bution. The effects of different parameters were evaluated,
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