Water Science and Engineering 2024, 17(1): 33e40

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Water Science and Engineering

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A prototype for on-site generation of chlorinated disinfectant for use in rural

aqueducts
Diana Marcela Cuesta Parra a,*, Felipe Correa Mahecha a, Andres Felipe Rubio Pinzon b,
Davidcamilo Ramírez Bustos b, Leonel Alveyro Teran Llorente c,
Miguel Fernando Jimenez Jimenez c
a
Chemical and Environmental Engineering Department, Fundacion Universidad de America, Bogota 117111, Colombia
b
Chemical Engineering Department, Fundacion Universidad de America, Bogota 117111, Colombia
c
Mecanical Engineering Department, Fundacion Universidad de America, Bogota 117111, Colombia
Received 17 January 2023; accepted 10 May 2023
Available online 29 May 2023

Abstract

Sodium hypochlorite has significant potential as a sanitation solution in hard-to-reach areas. Few studies have investigated the optimal
electrolysis parameters for its production with volumes greater than 10 L. This study evaluated sodium hypochlorite production through
electrolysis in a 22-L prototype and identified the optimal operating parameters. Tests were performed using graphite electrodes with areas of
68.4 cm2 at the laboratory scale and 1 865.0 cm2 at the prototype scale. A design for experiments with different operating times, chloride
concentrations, and electric current intensities was developed. The optimal operating time, sodium chloride concentration, and current intensity
at the laboratory scale were 120 min, 150 g of chloride per liter, and 3 A, respectively, leading to the production of 5.02 g/L of the disinfectant
with an energy efficiency of 12.21 mg of Cl2 per kilojoule. At the prototype scale, the maximum sodium hypochlorite concentration of 3.99 g of
chloride per liter was achieved with an operating time of 120 min, a sodium chloride concentration of 100 g of chloride per liter, and a current
intensity of 70 A, reaching an energy efficiency of 42.56 mg of Cl2 per kilojoule. In addition, this study evaluated the influences of the chloride
concentration, current intensity, and operating time on the production of sodium hypochlorite at the two scales, and formulated the equations
showing the trends of sodium hypochlorite production and energy efficiency in the electrochemical systems. The 22-L prototype model for
production of this oxidizing substance is promising for disinfection of large volumes of water in areas that are difficult to access.
© 2023 Hohai University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).

Keywords: Disinfection; Electrolysis; Energy efficiency; Optimization; Sodium hypochlorite

1. Introduction water sources (Khalid et al., 2020; Lin et al., 2022), generating
an increase in the biological demand for oxygen in rivers in
The presence of industrial, agricultural, and domestic waste various parts of the world (UN-Water, 2016).
in the environment is a growing problem for ecosystems and Around the world two billion people consume water
communities, because about 80% is directly discharged into contaminated with pathogenic microorganisms (World Health
Organization, 2022). It is estimated that 780 000 people died
from poor water sanitation by 2019 (UNESCO World Water
This work was supported by the America University, the Swiss Agency for Assessment Program, 2019). In Colombia, a study in 2022
Development and Cooperation, and the Central Technical Institute. conducted on 51.2% of municipalities concluded that 0.7% of
* Corresponding author.
the population did not have access to water meeting minimum
E-mail address: [email protected] (Diana Marcela
Cuesta Parra). quality standards for human consumption (National Institute
Peer review under responsibility of Hohai University. of Health, 2022).

https://doi.org/10.1016/j.wse.2023.05.005
1674-2370/© 2023 Hohai University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/
licenses/by/4.0/).
34 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40

Treatment is usually carried out with oxidizing agents, such the reagent system. Finally, tests were carried out in a proto-
as chlorinated species, which are the most commonly used for type using a 22-L electrochemical reactor built in Colombia.
disinfecting drinking water. These substances can be found in The prototype included a control board, where the values of
the form of molecular chlorine (Cl2), sodium hypochlorite process variables, such as pH, voltage, mixing time, and
(NaClO), hypochlorous acid (HClO) (Zaviska et al., 2012), or electric current supplied to the system, were observed. It also
calcium hypochlorite (Ca(ClO)2) (World Health Organization, had four electrodes connected in parallel, with a total sub-
2020). Some of them are obtained through electrolysis, a merged area of 1 865.0 cm2 and a spacing of 8 mm between
method easy to implement in areas that are difficult to access, plates.
such as Chad, creating solutions for sanitation problems in
rural areas (Campos Nogueira et al., 2021). 2.2. Experimental procedure
The process of hypochlorite production through electrolysis
is a widely studied technology. Hsu et al. (2015) produced a Saline solutions at chloride concentrations of 100 and 150 g
disinfectant solution from seawater with coated titanium of Cl
per liter were introduced into a beaker where elec-
electrodes, achieving process optimization and high yields trolysis was carried out up to a volume of 200 mL. As for the
towards the production of chlorine. Khalid et al. (2018) opti- electrode material (anode and cathode), graphite was used
mized the electrolysis process with the response surface with a gap of 8 mm and an anodic area of 68.4 cm2. This
methodology for production and process efficiencies, and the process was performed over different durations (30, 60, 90,
parameters of voltage, time, and electrolyte concentration and 120 min). Based on the chloride concentration (X1), time
were considered due to their importance in hypochlorite syn- periods (X2) of 60e120 min, and current intensity (X3) at
thesis. Other studies have found that the parameters affecting levels of 1, 5, and 3 A, a factorial design was developed to
the production of sodium hypochlorite in electrolysis cells are determine the optimal operating conditions at the laboratory
amperage (Ghalwa et al., 2012) or current density (Saleem scale. At the end of each test, the pH value of the solution was
et al., 2012), sodium chloride (NaCl) concentration measured with an Apera PH 700 reference potentiometer
(Ghasemian et al., 2017), time (Saha and Gupta, 2017), elec- (Ohio, USA).
trode spacing (Ronco and Mishkin, 2007), and electrolyte
type, and sodium chloride has been found to perform better in 2.3. Experimental process of prototype
the electrolysis process than other salts (Ghalwa et al., 2012).
Saha and Gupta (2017) evaluated the influence of graphite The process in the prototype was carried out using solutions
electrodes and found that the production of active chlorine is of 50 and 100 g of Cl
per liter made from Refisal® sodium
proportional to current density and time (Saha and Gupta, chloride (99% purity), and the synthesis of sodium hypo-
2017). chlorite was performed by configuring the control panel ac-
Girenko et al. (2021) used continuous flow systems with a cording to the operating conditions: an electrical current of
flow rate of 9.2 L/h and generated 1 g/L of disinfectant. They 40e70 A with a voltage of 4 V (Table 1). During the process,
demonstrated a low yield and high operating costs associated samples were taken at 60, 90, and 120 min. In these condi-
with the transport of the fluid, indicating that the batch sys- tions, a factorial design of experiments was developed to
tems achieved a higher concentration of disinfectant with determine the optimal operating conditions.
better energy efficiencies. This study aimed to evaluate the
production of a chlorinated disinfectant obtained through 2.4. Quantification of free chlorine
electrolysis in a prototype to identify the optimal parameters
of the electrolysis process (such as electrolysis time, NaCl The 4500-Cl B iodometric method from the standard
concentration, and electric current) as a function of hypo- methods of Baird et al. (2017) was used. Two aliquots of
chlorite production. The results of this study can be used to 10 mL of samples were taken after each electrolysis process to
find the operating parameters of 22-L electrolysis sodium quantify the amount of free chlorine in the samples per
hypochlorite generators with graphite electrodes to disinfect replicate (Baird et al., 2017).
large volumes of water in hard-to-reach areas.
2.5. Energy efficiency for hypochlorite production
2. Materials and methods
Energy efficiency was calculated according to Faraday's
2.1. Experimental set-up law, which establishes a relationship between the mass of a
substance released from an electrolyte during the passage of
In laboratory-scale tests, a 250-mL beaker, graphite elec- an electric current when these electrolysis processes are car-
trodes, and 200 mL of brine solution generated from Refisal® ried out (Hsu et al., 2017). Electrical power was calculated
sodium chloride (99% purity) were used. The electrodes were with Eq. (1) (Zaviska et al., 2012):
connected to an Extech® Instruments DCP60 reference power
supply (Nashua, USA) that regulated the voltage from 0 to PE ¼ VI ð1Þ
60 V, and electric current between 0 and 10 A was supplied to
 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40 35

Table 1
Summary table of parameters used at laboratory and prototype scales.
Scale Electric potential (V) Electrode gap (mm) Electrolyte volume (L) Electrode number Electrode material Electrode area (cm2)
Laboratory 4 8 0.2 2 Graphite 68.4
Prototype 4 8 22.0 4 Graphite 1 865.0

where PE is the electrical power (J/s), V is the voltage (V), and

I is the current (A). The electrical energy consumed in the Table 2
electrolysis process was estimated with Eq. (2): Electrical conductivity and electrical resistivity of different types of
electrodes.
PE TE Type of Electrical Electrical References
EE ¼ ð2Þ electrode conductivity resistivity
1 000
(S/m) (U$m)
where EE is the consumed electrical energy (kJ), and TE is the Graphite 1.0  105 1.00  10
6 Mitchell (2003);
electrolysis time (s). The produced total chlorine was calcu- Herbert et al. (2012)
lated with the iodometric method that uses the amount of Stainless steel 1.4  106 7.40  10
7 Mitchell (2003);
experimental chlorine and the volume of water used for Ralls et al. (1976)
Titanium 1.8  106 4.20  10
7 Ida (2013);
electrolysis (Hsu et al., 2017): Ralls et al. (1976)
Platinum 9.4  106 1.06  10
7 Ida (2013);
M ¼ rðClÞVw ð3Þ
Mitchell (2003)

where M is the amount of the produced total chlorine, r(Cl) is

Platinum and graphite were the main materials used to
the concentration of the experimental chlorine (mg/L), and Vw
carry out the process. The cost of these electrodes is important
is the volume of water used for electrolysis. The energy effi-
to consider for disinfection in areas difficult to access and with
ciency of electrolysis processes was evaluated through Eq. (4),
limited economic resources. The material that meets the
which involves the amount of the produced total chlorine and
desired characteristics is graphite, which is easily accessible
the electrical energy consumed through each electrolysis
and has a high resistance to degradation by corrosion, being
process (Khalid et al., 2018):
inert with electrolytes (Nurul Aniyyah et al., 2022). In recent
M surveys, dimensionally stable anode (DSA)-mixed metal oxide
RE ¼ ð4Þ
EE electrodes were used as catalysts to increase the yields in
electrochemical production of chlorine. High costs, lower
where RE is the electrical or energy efficiency of electrolysis selectivity, and detrimental effects on the environment have
processes (milligrams of Cl2 per kilojoule). limited the use of this technology (Wang et al., 2021).

3. Results and discussion 3.2. Evaluation at laboratory scale

The sodium hypochlorite concentration generated in each The electrochemical process for the production of sodium
experiment was evaluated at laboratory and prototype scales. hypochlorite involves a series of oxidation-reduction reactions.
The energy efficiency was determined, and the electrode ma- Initially, the poles generated by electrodes result in the formation
terials with the best performance were selected. of ions (Ronco and Mishkin, 2007), which react to form sodium
hypochlorite, sodium chloride, water, and other substances
3.1. Selection of anode and cathode materials (Portarapillo et al., 2020). Eqs. (5) through (7) show the reactions
at the anode, at the cathode, and in the solution, respectively:
According to the studies of Khalid et al. (2018, 2020) and
Hsu et al. (2015), electrical conductivity is a determining factor 2Cl
/ Cl2 þ 2e
ð5Þ
in the selection of electrodes for the generation of sodium hy-
pochlorite because it is proportional to the transport of ions 2H2 O þ 2e
/ H2 þ 2OH
ð6Þ
during the process. Another important property is electrical
resistivity. Al-Areqi et al. (2021) indicated that electrochemical 2NaOH þ Cl2 / NaClO þ NaCl þ H2 O ð7Þ
activation increases when the material has a low electrical re- Table 3 shows the results of the experiments, including the
sistivity, thus favoring the ion exchange of the solution for the concentration of sodium hypochlorite produced during the
production of sodium hypochlorite (Khalid et al., 2020). laboratory-scale electrolysis tests and the energy efficiency
Table 2 shows the properties of different materials. The calculated with Eq. (4). Statistical analysis was performed
characteristics of titanium and stainless steel mean that these with Statgraphics Centurion XVI.
electrodes have the two main properties needed to carry out The statistical analysis showed that current intensity (X3) and
hypochlorite production (Khalid et al., 2020). These materials the concentration of NaCl solution (X1) had p values of 0.028 6
show the capability for corrosion decomposition due to their and 0.045 2, respectively, less than 0.05. This indicated that these
high reactivity with the electrolyte (Nurul Aniyyah et al., 2022). two variables significantly influenced the electrolysis process,
36 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40

Table 3 Fig. 2 shows the response surfaces of the produced sodium

Factorial design of experiment matrix with experimental results at laboratory hypochlorite as functions of the concentration of chloride,
scale.
time, and current intensity. In the conditions of a current in-
Experiment X1 X2 X3 Concentration Energy tensity of 3 A, a chloride concentration of 150 g of Cl
per
(grams (min) (A) of sodium efficiency
of Cl
hypochlorite (milligrams
liter, and an operating time of 120 min, the maximum pro-
per liter) (g/L) of Cl2 duction of sodium hypochlorite was 5.02 g/L. This result was
per kilojoule) due to the fact that the relation between the chloride concen-
1 100 60 1.5 3.28 34.50 tration and current intensity was proportional to the hypo-
2 100 120 1.5 3.16 17.11 chlorite concentration, which was also observed in other
3 100 60 3.0 3.44 15.85 investigations. Teguia and Noumi (2021) used electrodes with
4 100 120 3.0 4.17 9.41 graphite alloys in the conditions of a sodium chloride con-
5 150 60 1.5 3.28 36.64
6 150 120 1.5 3.55 19.50
centration of 300 g/L, a current intensity of 1 A, and an
7 150 60 3.0 4.87 22.12 operating time of 60 min, and achieved a sodium hypochlorite
8 150 120 3.0 5.02 12.21 concentration of 18 g/L. According to Ganijonovich (2023),
similar relations were observed between variables by
increasing the salt concentration (5%e30%) to produce a
with a model fit level of 99.88% and a total error of 4.5  10
3. higher concentration of active chlorine in a 500-mL
Unlike other studied variables, time did not significantly influ- system with graphite electrodes. With low salt concentra-
ence the electrolysis process as the p value was 0.116 1. This tions (1e3 g/L) and an increase in the operating time (60 min),
indicated that no significant difference was observed in the final it was possible to generate up to 76.07 mg/L of active chlorine
hypochlorite concentration. This variable was not eliminated in a 500-mL cell using titanium electrodes (Isa et al., 2009). At
from the model because it increased the adjustment error. Thus, similar concentrations, Whangchai et al. (2013) produced
it is necessary to analyze the time at shorter intervals. 221.35 mg/L of hypochlorite for an operating time of 60 min
The combination (X1X2) was excluded from the model and demonstrated that extending the operating time favored
because it did not have a significant influence in this case. Ac- the generation of the disinfectant of interest. Jeong et al.
cording to Fig. 1, current intensity was the variable with the (2009) performed an electrolysis process for 10 min with a
greatest influence on the process as it limited the amount of en- current density of 17 mA/cm2, and achieved a chlorine con-
ergy in electron migration to produce the disinfectant compound. centration of 30 mg/L, demonstrating the influence of current
As the result of the design of experiments, the fitted density and time. In the conditions of a current intensity of
mathematical model obtained with Statgraphics Centurion 60 mA/cm2 and an operating time of 60 min, Song et al.
XVI was expressed by Eq. (8), which relates the production of (2019) used titanium electrodes in a 500-mL cell and
sodium hypochlorite to current intensity, time, and the con-
centration of chloride:

rðNaClOÞ ¼ 10:026 3
0:058 65X1
0:065 458 3X2

3:66X3 þ 0:000 485X1 X2 þ 0:032X1 X3 þ
0:031X2 X3
0:000 215 556X1 X2 X3 ð8Þ

where rðNaClOÞ is the concentration of the produced sodium

hypochlorite (g/L).

Fig. 1. Standardized Pareto chart for sodium hypochlorite production

at laboratory scale (X1, X2, and X3 represent sodium chloride con-
centration, time, and current intensity, respectively, and variables with Fig. 2. Response surfaces of laboratory-scale sodium hypochlorite
a vertical blue line crossing their bars are statistically significant). concentration.
 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40 37

achieved higher chlorine production (reaching 140 mg/L of

disinfectant) than the aforementioned investigations. New
catalysts have been investigated in these chlorinated agent
generation processes with graphite electrodes, which were
modified with cesium oxide. Compared to conventional
graphite electrodes, these electrodes inhibited the reduction of
the product of interest in the process, increased the concen-
tration of the disinfectant in a 1-L electrolysis cell, and
improved the process voltage required in electrolysis

(Alvarado-Avila et al., 2022).

3.3. Energy efficiency

The variance obtained from the designed experiments was

analyzed. Consequently, the two factors X2 and X3 were
determined. They had p values less than 0.05, indicating that
these variables directly affected the energy efficiency when
their magnitudes were modified. The adjusted coefficient of
determination (R2) value was identified to be 98.67%.
As shown in Fig. 3, the interaction between the sodium
chloride concentration and time, both of which have low im-
pacts on energy efficiency, was initially eliminated in order to
obtain a better fit of the model. The factors generating the
most significant changes were current intensity and time,
followed by the combination of these two factors and the so-
dium chloride concentration, which did not significantly affect Fig. 4. Response surfaces of energy efficiency at laboratory scale.
the energy efficiency of the process.
As shown in Fig. 4(a), the maximum energy efficiency of RE ¼ 99:4475
0:1675X1
0:67175X2
30:2X3 þ
the process at the laboratory scale appeared in the conditions
0:00186X1 X2 þ0:104667X1 X3 þ0:204333X2 X3

of a sodium chloride concentration of 150 g of Cl
per liter, an
operating time of 60 min, and a current intensity of 1.5 A. At 0:000826667X1 X2 X3 ð9Þ
low sodium chloride concentrations, the energy efficiency did When the system was configured according to the optimum
not decrease significantly. Fig. 4(b) shows the effects of cur- specifications, the energy efficiency was 36.24 mg of Cl2 per
rent intensity and time. An increase in these variables lowered kilojoule, with a sodium hypochlorite production of 3.28 g/L.
the energy efficiency. As a mathematical model of the Naderi and Nasseri (2020) reported a maximum efficiency of
experimental design, Eq. (9) derived from Statgraphics approximately 42 mg of Cl2 per kilojoule in the conditions of
Centurion XVI describes the behavior of the energy efficiency 63.42 g/L of sodium chloride, 15.73 V of voltage, and
as a function of three variables: 15.63 min of operating time using graphite electrodes with a
volume of 200 mL. Temperature is another variable that af-
fects energy efficiency because temperature exceeding 40 C
favors chlorate formation and leads to changes of 1 g/L in the
hypochlorite concentration (Ronco and Mishkin, 2007). These
results show that the energy efficiency generally decreases
when high values of time and current intensity are required.
Thus, a high hypochlorite composition cannot be obtained in
the conditions that favor the energy efficiency. Hsu et al.
(2017) found that the energy efficiency was equally affected
by time and voltage, a variable proportional to the current
intensity, and it was possible to obtain an efficiency of
approximately 47 mg of Cl2 per kilojoule with titanium
electrodes.

Fig. 3. Standardized Pareto chart of energy efficiency (X1, X2, and X3 3.4. Evaluation at prototype scale
represent sodium chloride concentration, time, and current intensity,
respectively, and variables with a vertical blue line crossing their bars The experiments listed in Table 4 were carried out to
are statistically significant). quantify the best operating conditions for the prototype. The
38 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40

Table 4
Factorial matrix of design of experiments with results in prototype.
Experiment X1 X2 X3 Concentration Energy
(grams of (min) (A) of sodium efficiency
Cl
per liter) hypochlorite (milligrams of
(g/L) Cl2 per kilojoule)
1 50 60 40 1.18 45.09
2 50 120 40 2.06 39.30
3 50 60 70 1.56 31.52
4 50 120 70 1.96 19.77
5 100 60 40 1.82 69.45
6 100 120 40 2.79 53.31
7 100 60 70 2.42 52.56
8 100 120 70 3.99 42.56

initial chloride concentration exhibited a less significant

impact on the energy efficiency but showed a significant in-
fluence on the sodium hypochlorite concentration. Thus, high
levels of the initial chloride concentration were set, and the
current intensity and time conditions were also adjusted.
As shown in Fig. 5, the variable with the most significant
effect on the production of sodium hypochlorite in the proto-
type was the initial sodium chloride concentration, with a p
Fig. 6. Response surfaces of sodium hypochlorite concentration.
value of 0.019 5 (less than 0.05). Time and current intensity
had less significant effects, with p values of 0.021 6 and
0.039 9, respectively. and indicates that higher values of the two variables favored
Fig. 6 shows that the variables that directly affected the the production of sodium hypochlorite. As shown in Table 4,
generation of the chlorinated disinfectant in the prototype higher efficiency values were achieved due to shorter oper-
were the sodium chloride concentration, time, and current ating times and lower current intensities delivered to the sys-
intensity. Baydum and Sarubbo (2022) used electrolyzers with tem. Saleem et al. (2012) used titanium, aluminum, stainless
a volume of 8 L, titanium electrodes and different types of steel, and zinc electrodes and tested the generation of a
brine solution, and found that a higher salt concentration in the chlorinated disinfectant in a system with a volume of 3 L.
medium favored the formation of chlorine. As shown in They found that the influence of the operating time lasted up to
Fig. 6(a), the generation of sodium hypochlorite was favored 50 min. Spasojevic et al. (2015) performed the electrolysis
by the increase in the NaCl concentration in the electrolysis process for 8 h and generated 0.2 mol/L of sodium hypo-
medium, and the highest concentration of the disinfecting chlorite in a volume of 5 L using titanium electrodes coated
agent was achieved in the zone with a sodium chloride con- with ruthenium and titanium oxides. They showed that under
centration of 100 g of Cl
per liter. Hsu et al. (2015) used a low electrical potential conditions, a shorter time was required
12.9-L cell with titaniumeplatinum electrodes and achieved a to reach the maximum concentration of hypochlorite. Hsu
maximum concentration of 9027 mg of Cl2 per liter with an et al. (2017) concluded that with lower voltages, a longer
energy efficiency of 23.4 mg of Cl2 per kilojoule. Fig. 6(b) time is needed to obtain the same results. In relation to the
shows the effects of the current intensity and electrolysis time volume of the system, de Matos et al. (2006) used a 25-L
electrolyte with a chloride concentration of 10 g/L and ach-
ieved a chlorine concentration of 0.33 g/L, which was a lower
production than the aforementioned studies. This indicated
that increasing the chloride concentration was a viable option
to avoid high electrical energy consumption.

4. Conclusions

With a focus on the production of sodium hypochlorite at

two scales, this study evaluated the effects of essential vari-
ables, such as current intensity, time, and chloride concentra-
tion, through an experimental design, and identified the
Fig. 5. Standardized Pareto chart of hypochlorite production in con- variables that contributed to the synthesis of sodium hypo-
structed prototype (X1, X2, and X3 represent sodium chloride con- chlorite with graphite electrodes. The results showed that the
centration, time, and current intensity, respectively, and variables with highest sodium hypochlorite production at the laboratory scale
a vertical blue line crossing their bars are statistically significant). was 5.02 g/L in the conditions of a sodium chloride
 Diana Marcela Cuesta Parra et al. / Water Science and Engineering 2024, 17(1): 33e40 39

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Declaration of competing interest and physical characterization at different electrolysing parameters. Food
Res. 2(6), 512e519. https://doi.org/10.26656/fr.2017.2(6).107.
The authors declare no conflicts of interest. Khalid, N.I., Sulaiman, N.S., Ab Aziz, N., Taip, F.S., Sobri, S., Nor-
Khaizura, M.A.R., 2020. Optimization of electrolysis parameters for green
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