Enhanced Chromium Removal From Tannery Wastewater Through Electroco - 2024 - Hel
Enhanced Chromium Removal From Tannery Wastewater Through Electroco - 2024 - Hel
Enhanced Chromium Removal From Tannery Wastewater Through Electroco - 2024 - Hel
Heliyon
journal homepage: www.cell.com/heliyon
Research article
A R T I C L E I N F O A B S T R A C T
Keywords: This study is focused on reducing total chromium level in tannery wastewater through the
Water pollution electrocoagulation process, in order to comply with the maximum permissible limits (MPL) and to
Coagulation determine the effects from its main operating factors. For this purpose, a batch electrocoagulation
Flocculation
reactor was manufactured using iron electrodes. Next, the response surface methodology was
Hydrogen gas
Maximum permissible limits
applied in the experimental design using a Box–Behnken design (BBD) with three factors: current
intensity, treatment time, and pH level. In addition, the total chromium removal percentage was
taken as a response variable. The corresponding statistical analysis revealed that the treatment
time, current intensity, and pH level variables were significant at a confidence level of P −
value < 0.05. Obtained in this study for a 99% total chromium removal were: current intensity (I)
= 2.9A, time (t) = 18.1 min, and pH = 5.6. Our results indicated that the electrocoagulation
process effectively removes total chromium from tannery effluents up to MPL values.
1. Introduction
One of the most critical concerns reported by the tanning industry is wastewater management since approximately 45 − 50 m3 of
effluents are produced per ton of tanned leather [1]. These wastewater effluents are characterized by high levels of pollutants, such as
the biochemical oxygen demand (BOD), chemical oxygen demand (COD), total suspended solids (SST), sulfides, and chromium.
The tanning process that produces high pollution load can be divided into three stages: the beamhouse stage, the tanning stage, and
the finishing stage. In the beamhouse stage, the leather is prepared for crosslinking the tanning agent. In this stage, the salt used for
preserving the skin is removed, any remnants of hair and meat are removed, and the leather is divided to meet the desired thickness,
thereby producing a high organic load and chlorides in the effluents. In the tanning stage, the decalcifying agents and the remains from
proteins other than collagen are removed, and the skin is brought to an acidic pH level so that basic chromium sulfate can be cross
linked to collagen, the main tanning agent used in Peru as well as the most prominent pollutant in these effluents. Subsequently, the
* Corresponding author.
E-mail addresses: [email protected] (E. Aguilar-Ascón), [email protected] (L. Marrufo-Saldaña), [email protected] (W. Neyra-
Ascón).
https://doi.org/10.1016/j.heliyon.2024.e24647
Received 10 August 2023; Received in revised form 21 December 2023; Accepted 11 January 2024
Available online 23 January 2024
2405-8440/© 2024 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
E. Aguilar-Ascón et al. Heliyon 10 (2024) e24647
leather is retanned, dyed, and oiled to improve its physicomechanical properties. The last stage is finishing; the leather is given its final
appearance using resins, waxes, polymers, and lacquers, which are based on organic and aqueous solvents, thus generating emissions
mainly into the atmosphere (Fig. 1). Several research studies have already focused on finding chromium removal alternatives. This
pollutant comes from using basic chromium sulfate as a tanning agent. In the environment, the most stable forms of chromium are in
oxidation state (III) and (IV) Hiller et al., 2020 [2]. Chromium (III) is characterized by its oxidation capacity under certain envi
ronmental conditions, which in turn determines its ecotoxicity; even though in small concentrations, it is part of the metabolic pro
cesses of plants, animals, and humans. Nevertheless, chromium (III) in high concentrations and in its IV oxidation state is dangerous
because it is able to penetrate cell membranes via diffusion through ion channels. Studies have shown that a concentration > 10 mg/ L
Cr(III) in culture medium and concentrations of > 50 mg/Kg Cr(VI) in soil limit the germination of seeds of plant species [3]. Likewise,
it has been determined that Damage to DNA, in human being, may be caused by Cr (VI) at 0.2 mg/mL and Cr (III) at 0.1 mg/ mL [4].
The negative environmental impact of tanning has been widely studied and evidenced and therefore this industry is considered one
of the most polluting [5–8]. The pollutant load of their effluents is characterized by high levels of DOC, BOD, sulfides, TSS, chromium,
ammonia nitrogen among others [5,9]. In Peru, Supreme Decree No. 010-2023-minam updated the maximum permissible limits for
tannery effluents; however, compliance with these limits is a challenge because most companies, mainly SMEs, do not have efficient
treatment systems. In regions of Peru, such as Arequipa and Trujillo, tanneries are located around a body of water and there is a general
request for the development of common treatment plants, while in the Lima region, tanneries are atomized and need to move from
sedimentation ponds to technological solutions that minimize the pollutant load. Sewage sludge can be managed by disposal in
controlled landfills, but it is possible to recover chromium and use the remaining organic matter as a source for biogas production or as
material for composting [10].
The electrocoagulation process consists of applying an electrical current to two electrodes. Herein, one electrode acts as a sacrificial
anode and the other as a cathode [11,12]. This produces metal ions that allow the formation of coagulants on site by electrochemical
dissolution at the sacrificial anode without adding chemicals Lu et al., 2021 [13]. The cathode releases hydrogen gas by reducing H2 O
and the oxygen generated at the anode leads to a flotation process that causes suspended particles in the wastewater to rise to the water
surface [13,14]. The most commonly used electrode materials are iron (Fe ) and aluminum [15]. The mechanisms below describe the
formation of iron hydroxides. Equations (1)–(4) show the mechanisms describing the formation of iron hydroxides.
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E. Aguilar-Ascón et al. Heliyon 10 (2024) e24647
Fe − 2e→Fe2+ (1)
At alkaline conditions
Table 1
Articles related to this study.
Item Artículo Tipo de agua Material Concentración Eficiencia de Costo Consumo Referencia
de inicial de cromo eliminación (US$ /m3 ) de energía
electrodos Cri (mg/L) de cromo (%) (kWh /m3 )
1 Optimized Total Chromium Tannery Fe–Fe 121.35 99.9 0.223 0.58 Aguilar (2021)
Removal from Tannery wastewater
Wastewater using
Electrocoagulation and Iron
Electrodes: Application of the
Box Behnken Design (BBD)
2 Treatment of raw tannery Tannery Fe–Fe 570 99.7 0.70 Can be Deghles, A., &
wastewater by wastewater calculated Kurt, U. (2015)
electrocoagulation technique:
optimization of effective
parameters using Taguchi
method
3 Influence of experimental Tannery Fe–Fe 75 y 32 99 2.01 see Aboulhassan,
parameters in the treatment of wastewater M. A. et al.,
tannery wastewater by (2018)
electrocoagulation
4 The investigation of chemical Tannery Fe–Fe 400 ± 20 98.2 4.84 see Sari, (2018)
coagulation and wastewater
electrocoagulation processes
for tannery wastewater
treatment using response
surface methodology
5 Organic and inorganic matter Tannery Al–Al 2000–2300 98 0.8817 2.37 Bing, (2022)
removal from tannery wastewater
wastewater using the
electrocoagulation process
6 Treatment of highly Tannery Al–Al 7000 98.1 (dilución More than More than Elabbas S.
concentrated tannery wastewater 1:6) 20 20 et al., (2016)
wastewater using (tanning
electrocoagulation: Influence process)
of the quality of aluminium
used for the electrode
7 Reduction of turbidity and Al–Al 236.62 93 More than 41.36 Mounir Z,
chromium content of tannery 20 (2018)
wastewater by
electrocoagulation process.
8 Chromium removal from Tannery Fe–Fe 82.7 99.64 0.0277 to 0.333 to Patel, S., &
industrial effluent by wastewater 0.207 2.499 Parikh, S.
electrocoagulation: Operating (2021)
cost and kinetic analysis
9 Electrocoagulation of Tannery (Fe + Ti)– 10.0 99.16 – – Guiju Li,
chromium in tannery wastewater C (2019)
wastewater by a composite
anode modified with
titanium: parametric and
kinetic study
10 Enhanced treatment of Tannery Al-Al 30.11 39.79 – – Moradi, M., &
tannery wastewater using the wastewater Moussavi, G.
electrocoagulation process (2018)
combined with UVC/VUV
photoreactor: Parametric and
mechanistic evaluation.
11 Environmental impact Tannery Acero 3844 ± 1200 99.99 – – El-Khateeb,
elimination of chrome tanning wastewater (2017)
effluent using
electrocoagulation process
assisted by chemical oxidation
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E. Aguilar-Ascón et al. Heliyon 10 (2024) e24647
At acidic conditions
The raw tannery wastewater used in our experiment was supplied by Centro de Innovación Tecnológica del Cuero y Calzado e
Industrias Conexas (CITEccal is the Spanish acronym) from their pilot tanning effluent treatment plant. The wastewater sample was
taken at the outlet of the tanning plant settling tank in order to remove the larger particles. This water presents very similar char
acteristics to that produced by the tanning industry, as indicated in Table 2. In addition to high concentrations of organic matter and
chromium, this water also exhibits high conductivity values, which demands higher electrical current.
For these purposes, a batch reactor with the following dimensions was used: length: 30 cm ; width: 20 cm; and height: 25 cm. In
total, we used eight iron electrodes that worked as anodes and cathodes: each of them was 10 cm wide and 10 cm long, with a total area
of 100 cm2 . The electrodes were completely submerged in the wastewater. In the reactor the height of the water was 20 cm leaving 5 cm
free space for the accumulation of sludge. Due to the high conductivity values, we used a serial configuration of the electrodes with a
spacing of 2 cm to reduce electric current demands within. Power was supplied from a 0 − 24 V power source, with current range of
0 − 10 A (See Fig. 2).
The experiments were done under three different conditions of pH (8.5, 7, and 5.5), current intensity (1,2, and 3 A), and treatment
time (7, 14, and 21 min). To measure pH, conductivity and temperature, an Oakton PCS 35 multiparameter was used. In addition, the
following method was used to quantify total chromium (response variable): EPA 200.8 : 1994 Rev 5.4. Determination of Trace Ele
Table 2
Physicochemical effluent analysis.
Parameter Value LMP
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Fig. 2. Diagram of the electrocoagulation reactor with serial electrodes; (1) electrocoagulation cell, (2) power source, (3) iron electrodes (cathode
and anode), (4) sampler, (5) wastewater, (6) DC ammeter.
ments in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry. To determine the percentage of total chromium
removal, Equation (5) was used.
For total chromium:
( )
Cri − Crf
Yn = %R = x100 (5)
Cri
where:
%R : Percentage of total chromium removal.
The response surface method (RSM) is a methodology used for developing optimization models and processes [23]. As depicted in
Equation (6) below, RSM represents independent parameters quantitatively.
y = f (x1 , x2 , x3 , …, xn ) ± ε (6)
where y is the dependent variable (response parameter), f is the response function, ε is the experimental error, and x1 , x2 , x3 , …, xn are
the independent parameters.
The relationship between the independent and dependent variables is illustrated in Equation (7) below using a quadratic model.
y = β0 + β1 x1 + β2 x2 + β3 x3 + β11 x21 + β22 x22 + β33 x23 + β12 x1 x2 + β13 x1 x3 + β23 x2 x3 (7)
where β0 is the intercept; β1 , β2 and β3 are the linear coefficients; β11 , β22 and β33 are the quadratic coefficients; and β12 , β13 and β23 are
the interaction coefficients.
A Box–Behnken experimental design was used to find the main effect on total chromium removal from the operational factors, and
to determine the operational factor values that reach maximum chromium removal efficiency. To perform our statistical analysis, we
used the Design Expert 11.1 software, which reported an analysis of variance (ANOVA) table at a 95% confidence level, and the quality
of fit of the polynomial model was expressed by the coefficient of determination: R2 and Radj . The experimental design had three
factors, three levels, and thirteen experiments with two central points. The factors considered as independent variables were electric
current intensity (x1 ), treatment time (x2 ), and pH (x3 ). As a response variable, we used the percentage of total chromium removal (y1 )
(shown in Table 3).
Table 3
Independent variable ranges and their levels.
Factor Variables Levels
− 1 0 +1
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The results from total chromium removal expressed as the variable and response by the electrocoagulation were proposed ac
cording to the design matrix in Table 4. The Box–Behnken design included 13 experiment sets and 2 core experiments. The statistical
analysis was performed using Design Expert 11.1 software. Using multiple regression analysis, the chromium removal percentage
response variable (y1 ) was correlated with three design factors (x1 , x2 , x3 ) using the second order polynomial (Eq. (7)). Table 5 below
presents the quadratic regression model for total chromium removal (y1 , %), in terms of coded factors.
The adequacy of the total chromium removal model using iron electrodes was also verified based on the regression coefficient R2 ,
the adjusted R2 value, the predicted R2 value, the F value, and the P − values (see Table 5).
In addition, an ANOVA yielded a 95% confidence level, comparing the variation sources against Fisher’s distribution (F − test) to
validate the viability of the regression model. The regression coefficient (R2 ) is an important parameter for validating model adequacy
and this value must be at least 0.80 for the model to be a good fit [24]. In this study, the R2 value for total chromium removal with iron
electrodes is R2 = 0.9796, which demonstrates a good model adequacy. The adjusted R2 and predicted R2 values were 0.94 and 0.56,
respectively, as shown in Table 6. The predicted R2 values are the values predicted by the design, which measures the variation of the
data predicted by the model. The results reveal that the time, current intensity, and pH variables were significant based on the response
variable (y) at a confidence level of P − value < 0.05.
Fig. 3 denotes both the experimental and predicted values from our model. Here, both the observed and obtained values are very
close to linearity, thereby indicating that both values are accurate and reliable.
Current intensity is the most important parameter in the electrocoagulation process as it controls both coagulant dosing rates and
reaction rates within the medium [25]. As current intensity increases, the amount of anodic iron dissolution also increases, which leads
to better coagulation. However, very high current intensity values applied for a long time may decrease efficiency due to oxygen
production and the passivation of the electrodes [26]. For the treatments, current intensities of 1, 2, and 3 A were used. As shown in
Fig. 4a y 4b, the percentage of total chromium removal increases as current intensity increases. The foregoing happens because current
intensity produces anodic dissolution of iron and generates hydroxocationic complexes or iron hydroxide, which, due to surface
complexation and electrostatic attraction [25,27], agglomerate particles and remove pollutants [28]. This is reflected in the results
from applying 2 and 3 A, with which 94% efficiency is achieved after 14 min of treatment. This result is lower than the values reported
by Genawi, who achieved an efficiency close to 100% using iron electrodes and applying current densities of 13 mA/cm.2 [20].
El-Taweel also reported obtaining maximum efficiency using iron electrodes at 1 A for 15 min. These results were justified because
these experiments used synthetic water [17]. Furthermore, Deghles obtained a higher 99% efficiency at a current density of 30 mA/
cm.2 and a treatment time of 25 min [28].
Several studies have demonstrated that pH modifies surface particle charges and affects the speciation of iron species, thus
significantly influencing the electrocoagulation process mechanism [24,26]. Metal hydroxide precipitations are controlled by pH level
Table 4
Box–Behnke design for chromium removal.
Exp. No Factors Chromium Removal (%)
Current intensity (A) Treatment Time (min) pH Actual value Predicted value
x1 x2 x3 y1 a y1 p
1 2 21 5.5 92 96
2 2 21 8.5 27 33
3 2 7 8.5 18 14
4 1 14 8.5 17 14
5 1 7 7 26 33
6 2 14 7 27 27
7 1 21 7 38 35
8 3 21 7 71 64
9 3 14 5.5 94 97
10 2 14 7 26 27
11 1 14 5.5 85 84
12 3 7 7 31 34
13 3 14 8.5 31 32
14 2 7 5.5 91 85
15 2 14 7 28 27
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Table 5
Statistical parameters obtained using RSM for chromium removal (%).
Response R2 Adj − p Quadratic Response Model based on Least Squares
R2
(%) (%)
Chromium 0.9796 0.9428 0.0011 ya = 762.22222 − 40.70833x1 − 6.44048x2 − 167.52778x3 + 1.0000x1 x2 + 0.833333x1 x3 +
Removal (%) 0.190476x2 x3 + 7.12500x21 + 0.150510x22 + 10.05556x23
(Chromium removal, %); ya (Current intensity, A); x1 (Time, min); x2 (pH); x3
Table 6
ANOVA table.
Source Sum of Squares DF MS F Value P-Value
Fig. 3. Regression plot illustrating the correlation between experimental data and predicted values obtained using the response surface method
ology, describing percentage removal of chromium.
variations, which remove pollutants and agglomerate coagulants when acting as coagulants [27]. The Fe3+ generated will undergo
immediate reactions producing several monomeric or polymeric metal complexes, such as Fe (OH)3 , Fe (OH)−4 , Fe (H2 O)3 (OH)3 ,
Fe (H2 O)3+ 4+ 2+
6 ,Fe (H2 O)5 (OH)2 ,Fe (H2 O)4 (OH)2 ,Fe (H2 O)8 (OH)2 , and Fe2 (H2 O)6 (OH)4 [29]. These compounds remain in the medium as
+ +
an aqueous suspension, which can remove pollutants from wastewater by coagulation within a pH range of 2 − 6 [27,29]. To
determine the effects of pH on total chromium removal, we used pH valsues between 5.5 and 8.5 in this study. In Fig. 4b y 4c, shows
that the best efficiencies were obtained at pH = 5.5, where a maximum chromium removal value of 94% was achieved with a current
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E. Aguilar-Ascón et al. Heliyon 10 (2024) e24647
Fig. 4. Three-dimensional and contour response surface charts for biochemical oxygen demand removal percentages a) current intensity and
treatment time; b) current intensity and pH level; and c) treatment time and pH level.
intensity of 3 amperes and a time of 14 minutes. This result is consistent with the values reported by Shahriari, who obtained the
highest chromium removal efficiency at an optimum pH of 6 , who reported that the hydroxide produced formed a gelatinous sediment
of iron hydroxide and then a cosediment of iron and chromium was formed [30]. Chromium (+3) at acidic pH, lower than 3, remains in
its ionic form, as OH- radicals increase, they form complexes with chromium, reaching higher pH, this causes the precipitation of
chromium hydroxide (Covarrubias, C. et al. ,2005; Basaldella, E, 2007). In addition, Golder reported that the optimum pH for chro
mium removal in monopolar and bipolar configurations was 6 and 5.5, respectively [31]. Furthermore, Genawi indicated that, when
using iron electrodes, the maximum chromium removal efficiency occurred at pH values close to 7 [21]. In contrast, Deghles reported a
99% chromium removal efficiency at pH levels of 7 − 8 when using iron electrodes [28]. However, during the experiments, a
disadvantage of using iron electrodes was observed; the treated water turned black due to the reaction of Fe2+ , Fe3+ , and H2 S, HS− , S−2 ,
which generated a black Fe S precipitate [32].
Treatment times have a direct effect on electrocoagulation process efficiencies [33]. This parameter influences the production rate
of coagulant, OH− , and H2 , as well as affects the cost-effectiveness of the process [33,34]. Hence, we varied the treatment time in the
range of 7 − 21 min.
As shown in Table 3 and Fig. 4a y 4c, the results from this parameter confirm that the total chromium removal efficiency increases
over the course of treatment time. It is observed that at a treatment time of 7 min, the lowest efficiency values are obtained, ranging
from 17% to 31%. On the other hand, at 7 and 14 minutes of treatment at a pH of 5.5, 90% efficiency is exceeded. This is very similar to
the values reported by El-Taweel, where the processes reach their maximum chromium removal efficiency after 14 min [17]. However,
these values are not consistent with Deghles, whose processes achieved their best efficiency at 25 min of treatment [23]. Furthermore,
De la Luz-Pedro reports treatment times > 60 min for the removal of chromium [35]. Hence, we must determine our optimal treatment
time because very long treatment times lead to high electrode and energy consumption [36].
The Box–Behnken response surface methodology was used for numerical optimization to determine the optimal parameters to
maximize total chromium removal efficiency (y). The effects of the process variables are shown in Fig. 4a,b,c, which represent the
three-dimensional and contour (two-dimensional) response surface plots, which use the mathematical models developed in Equation
(7), wherein chromium removal percentage variations may be observed, according to the variation of their current intensity (x1 ),
treatment time (x2 ), and pH level (x3 ), factors. The optimization model predicted the following parameters for optimal conditions:
current intensity 2.9 A, pH = 5.6, and treatment time 18.1 min. Under these conditions, 99.9% total chromium removal efficiency was
achieved.
The operation costs for laboratory scale units are estimated considering energy costs and the quantity of materials and chemicals
consumed. Herein, the operation costs were calculated as follows:
CopT = Cop1 + Cop2 (8)
where, CopT represents total operation costs, Cop1 the electrode consumption operation costs, and Cop2 the energy consumption
operation costs. Rewriting Equation (8) explicitly:
CopT = ρelectrodes x ωelectrodes + ρenergy x βenergy (9)
where, ρelectrodes represents the price of the electrode material, and ωelectrodes the consumed electrode material weight, which could be
estimated as follows:
ωelectrodes = ηc x ωc + ηa x ωa (10)
where, ωelectrodes represents the total electrode weight, ηc the number of cathodes, ηa the number of anodes, ωc the cathode weight (g),
and ωa the anode weight (g).
While ρenergy represents the price per energy unit, and βenergy (kWh /m3 ) is the energy consumed. The latter is calculated as follows:
UxIxt
Ce = (11)
V x 1000
where, Ce represents the energy consumption (kWh /m3 ), U is the potential (V), I is the current (A), t is the treatment time ((h), and V is
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4. Conclusions
This study shows that electrocoagulation with iron electrodes is effective in reducing total chromium from raw tannery wastewater.
According to the experimental design results, current intensity, treatment time, and pH levels are crucial for total chromium removal.
The high R2 = 0.9796 and adj R2 = 0.9428 values confirm a good fit of the model used for total chromium removal. To achieve 99%
efficiency in the removal of total chromium, a current intensity (I) = 2.9 A, time (t) = 18.1 min and pH = 5.6 should be used. Based on
these results, we infer that changing the pH level of the effluent helps in obtaining the highest possible efficiency using iron electrodes.
It is also important to note that iron electrodes cause treated tannery water to turn black, which originates from the reactions between
iron ions and sulfide compounds. The data obtained in this study allow us to have relevant information for future designs of pilot or
larger scale plants and thus define an optimal treatment ril to solve the environmental problem generated by the effluents of the
tannery industry. In addition, it is proven that electrocoagulation is efficient for chromium removal; however, due to the character
istics of the effluent, it is recommended to add other technologies such as advanced oxidation and filtration to comply with the
environmental standard.
Edwar Aguilar-Ascón: Writing – review & editing, Supervision, Methodology, Investigation, Conceptualization. Liliana Marrufo-
Saldaña: Writing – review & editing, Methodology, Formal analysis. Walter Neyra-Ascón: Writing – review & editing, Visualization,
Software.
First of all, I would like to greet you and hereby state that all the authors who have participated in the preparation of this article
have no conflict of interest and agree with the regulations of the journal.
Acknowledgements
The authors would like to express their gratitude to the Institute for Scientific Research at the Universidad de Lima for promoting
the comprehensive development of this project. Furthermore, the authors would also like to thank the Centro de Innovación Productiva
y Transferencia Tecnológica del Cuero y el Calzado (CITEccal Lima).
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