Voltammetric Studies Research Articles

Electrochemical Activity of Pure and Sn-Doped CeO<sub>2</sub> Nanoparticles using Simple Chemical Precipitation Method

In the present work, pure and Sn-doped CeO2 nanoparticles (NPs) were synthesized by the chemical precipitation method calcined at 400 ºC for 4 h. Characterization of NPs was done through X-ray diffraction (XRD), UV-visible, photoluminescence (PL), Fourier transform infrared (FTIR) spectroscopy and high-resolution electron microscope (HRTEM) techniques. The XRD study revealed the crystalline nature, size, and structure of the prepared NPs. The HRTEM results illustrated cubic structure. The UV–visible and PL studies were used to measure the optical behaviors of CeO2 NPs. The UV-visible showed that the bandgap value of CeO2 NPs increased from 3.61 to 3.65 eV for different doping concentrations. The XRD study exhibited that the size of the CeO2 NPs reduced from 11.03 to 7.91 nm. From the TEM analysis, the average size of undoped and 10% Sn-doped CeO2 NPs was calculated as 9.3 and 7 nm, respectively. A cyclic voltammetric study confirmed that Sn-doped CeO2 exhibited a higher specific capacitance value than the pure CeO2. The chemical precipitation method observed excellent redox and oxidation behavior were observed for Sn-CeO2 NPs by the cyclic voltammetric study. The significant enhancement in the specific capacitance suggested that Sn-doped CeO2 is a promising material for supercapacitor applications.

Electrochemical studies of catechol and hydroquinone at poly(nigrosine) modified carbon paste electrode: a cyclic voltammetric study

Electrochemical studies of catechol and hydroquinone at poly(nigrosine) modified carbon paste electrode: a cyclic voltammetric study

A low-cost carbon-based electrochemical platform for determining 2,3-dihydroxyphenol: applications in natural water and biodiesel samples.

2,3-Dihydroxyphenol (DHP) is a phenolic compound that has been used as an additive in biodiesel to avoid the auto-oxidation of biofuels and also in the production of cosmetic products. However, this substance can be released into the environment during its manufacture, transport, disposal and industrial use and can be harmful to health due to its toxicity, and hence, monitoring its presence in different samples is very important. Therefore, this work describes an electroanalytical study of DHP using different carbon-based pastes prepared to evaluate which one would be more promising to be used as an electrochemical platform for DHP quantification. The materials studied (graphite, carbon black and carbon nanotubes) in this work were characterized by Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy and the Boehm method. Voltammetric studies showed that pure carbon black presented a higher current density for detecting DHP than the other materials tested (graphite, carbon black + graphite, carbon nanotubes, carbon nanotubes + graphite). In studying the medium's pH, the highest currents occurred in acid media and acetate buffer solutions. After optimizing the experimental parameters, it was possible to obtain a wide range of linear responses from 0.1 to 10 000 μmol L-1 for DHP and a good limit of detection (LOD) of 0.03 μmol L-1. The selectivity of the electrode was tested for different species that may be present in samples containing DHP. Finally, the electrode was applied to determine DHP in natural water and biodiesel samples, showing recovery values between 98 and 102%, indicating good accuracy.

Detection of Residual 2-Phenylphenol on Lemon Rind by Electrochemically Deposited Poly(hydroxybenzaldehyde) and Poly(hydroxybenzoic acid) Polymeric Stackings as Electrode Modifiers

This study explores the characteristics of electrodeposition of the three hydroxybenzaldehyde isomers and selected hydroxybenzoic acids (4-hydroxybenzoic acid, salicylic acid, 3,5-dihydroxybenzoic acid) from mesityl oxide solvent. Similar to recent advances of this solvent, used by electrochemical studies, the carbon-carbon double bond had significant influence on the formation of polymers from the outlined molecules. In case of most substrates the peak currents increased to a steady-state but electropolymerization of some substrates caused significant deactivation. Scanning electron microscopic and complementary voltammetric studies facilitated that the electrochemically formed polymers are present on the electrode surface in stackings. In viewpoint of analysis of 2-phenylphenol, the modifying deposit formed from 4-hydroxybenzaldehyde was the best with 5 µM detection limit obtained with differential pulse voltammetry. Furthermore, a new procedure was chosen for the involvement of a cavitand derivative into the organic layers with the purpose to improve the layer selectivity (subsequent electrochemical polymerization in an other solution). Further studies showed that in this way the sensitivities of as-modified electrodes were a little worse than without this step, thus indicating that application of this step is disadvantageous. Recovery studies of 2-phenylphenol were carried out on lemon rind without any treatment, and it was compared with the case when the outer yellow layer was removed by rasping. The inner tissues showed very high adsorption affinity towards 2-phenylphenol.

Sensitive and Selective Voltammetric Sensor Based on Anionic Surfactant-Modified Screen-Printed Carbon for the Quantitative Analysis of an Anticancer Active Fused Azaisocytosine-Containing Congener

3-(4-Nitrophenyl)-8-(2,3-dimethylphenyl)-7,8-dihydroimidazo[2,1-c][1,2,4]triazin-4(6H)-one (NDIT) is one of the most promising candidates for anticancer agents. Hence, a sensitive and selective sodium dodecyl sulfate-modified screen-printed carbon sensor (SPCE/SDS) was used for its quantitative analysis. The SPCE/SDS, in contrast to the SPCE, showed excellent behavior in the electrochemical reduction of NDIT by differential-pulse adsorptive stripping voltammetry (DPAdSV). Cyclic voltammetric (CV) studies reveal an irreversible, two-stage and not purely diffusion-controlled reduction process in 0.01 M HNO3. The sensor was characterized by CV and electrochemical impedance spectroscopy (EIS). Under the optimized conditions (t 45 s, ΔE 175 mV, ν 150 mV/s, and tm 5 ms), the DPAdSV procedure with the SPCE/SDS presented a very wide linear range from 1 to 2000 nM and a low detection limit of 0.29 nM. A 1000-fold excess concentration of potential interferents commonly present in biological samples did not significantly alter the peak current of NDIT. The practical application of the proposed DPAdSV procedure with the SPCE/SDS was successfully checked by analyzing spiked human serum samples.

Voltammetric and Fluorimetric Studies of Dibenzoylmethane on Glassy Carbon Electrodes and Its Interaction with Tetrakis (3,5-Dicarboxyphenoxy) Cavitand Derivative

Due to the medical importance of dibenzoylmethane, one of the aims of the study was to find an appropriate packing material and a biologically friendly co-solvent to help its introduction into living systems. Accordingly, redox properties of dibenzoylmethane were investigated on glassy carbon electrodes in acetonitrile and in 1-propanol with cyclic voltammetry, and showed a diffusion-controlled process. In the anodic window, an oxidation peak appeared at around 1.9 V in both solvents. Cycling repeatedly between 0 and 2 V, the reproducibility of this peak was acceptable, but when extending the window to higher potentials, the electrode deactivated, obviously due to electrode material. The addition of the investigated tetrakis(3,5-dicarboxyphenoxy) cavitand did not significantly change the voltammograms. Further electrochemical experiments showed that the coexistence of water in acetonitrile and 1-propanol drastically reduces the solubility of dibenzoylmethane. Moreover, very rapid electrode deactivation occurred and this fact made the use of electrochemical methods complicated. Considering that both the cavitand and dibenzoylmethane are soluble in dimethyl sulfoxide, the interaction of these species was investigated and formation of stable complexes was detected. This observation was verified with fluorescence quenching studies. The mixture of water and dimethyl sulphoxide also dramatically improved the solubility of the cavitand-dibenzoylmethane complex at high excess of water. The addition of cavitand improved the solubility of dibenzoylmethane, a property which supports the application of dibenzoylmethane in therapy.

Molecularly Imprinted Polymer-Based Electrochemical Sensor for Rapid and Selective Detection of Hypoxanthine.

In this paper, we report on the coupling of an electrochemical transducer with a specifically designed biomimetic and synthetic polymeric layer that serves as a recognition surface that demonstrates the molecular memory necessary to facilitate the stable and selective identification of the meat-freshness indicator hypoxanthine. Consumer preferences and the food safety of meat products are largely influenced by their freshness, so it is crucial to monitor it so as to quickly identify when it deteriorates. The sensor consists of a glassy-carbon electrode, which can be regenerated in situ continuously, functionalized with molecularly imprinted polymers (MIPs) and a nanocomposite of curcumin-coated iron oxide magnetic nanospheres (C-IO-MNSs) and multiwalled carbon nanotubes (MWCNTs) that enhance the surface area as well as the electroactive characteristics. The electrochemical behavior of the fabricated sensor was analyzed by both cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Differential pulse voltammetric studies revealed the rapid response of the proposed sol-gel-MIP/MWCNT/C-IO-MNS/GCE sensor to hypoxanthine in a concentration range of 2-50 µg/mL with a lower limit of detection at 0.165 μg/mL. Application of the newly fabricated sensor demonstrated acceptable recoveries and satisfactory accuracy when used to measure hypoxanthine in different meat samples.

Voltammetric and electrodeposition study for the recovery of antimony from effluents generated in the copper electrorefining process

Antimony is a metalloid with limited availability as a primary resource, but it is commonly found as an impurity in effluents generated in the copper metallurgy. Thus, the development of clean and selective processes to recover antimony from these wastewaters would improve the sustainability of the copper production. In this work, an emulated effluent of the copper electrorefining industry that contains antimony and hydrochloric acid was characterized by means of voltammetric and electrodeposition tests using two different cell configurations: a static cell, and a dynamic cell with a rotating disk electrode (RDE). Voltammograms were obtained at varying hydrochloric acid and antimony concentrations, inversion potentials, scan rates and RDE rotation rates. Two main conclusions were drawn: (a) the deposition of antimony is a mass transfer-controlled process; and (b) an increase in hydrochloric acid concentration improves the deposition of antimony. The diffusion coefficient of antimony species was obtained applying the Randles-Ševčík and the Levich equations; both of them providing very similar values (5.29 ± 0.20 · 10−6 cm2 s−1). The effective electrodeposition of antimony from highly concentrated hydrochloric acid solutions was demonstrated. The surface examination of the electrodes revealed that compact and adherent deposits of antimony could be obtained under operating conditions that minimize the hydrogen evolution reaction in both potentiostatic and galvanostatic modes. Intensified convective regimes by using the RDE improve the supply of dissolved antimony towards the electrode surface, thus leading to a notorious increase in current density and, consequently, in the rate of antimony deposition.

Voltammetric Study and Modeling of the Electrochemical Oxidation Process and the Adsorption Effects of Luminol and Luminol Derivatives on Glassy Carbon Electrodes.

Luminol is one of the most widely used electrochemiluminescence (ECL) reagents, yet the detailed mechanism and kinetics of the electrochemical oxidation of luminol remain unclear. We propose a model that describes the electrochemical oxidation of luminol as multiple electron transfer reactions followed by an irreversible chemical reaction, and we applied a finite element method simulation to analyze the electron transfer kinetics in alkaline solutions. Although negligible at higher pH values, the adsorption of luminol on the glassy carbon electrode became noticeable in a solution with pH = 12. Additionally, various types of adsorption behaviors were observed for luminol derivatives and analogues, indicating that the molecular structure affected not only the oxidation but also the adsorption process. The adsorption effect was analyzed through a model with a Langmuir isotherm to show that the saturated surface concentration as well as the reaction kinetics increased with decreasing pH, suggesting a competition for the active sites between the molecule and OH-. Moreover, we show that the ECL intensity could be boosted through the adsorption effect by collecting the ECL intensity generated through the electrochemical oxidation of luminol and a luminol analogue, L012, in a solution with pH = 13. In contrast with luminol, a significant adsorption effect was observed for L012 at pH = 13, and the ECL intensity was enhanced by the adsorbed species, especially at higher scan rates. The magnitude of the enhancement of the ECL intensity matched well with the simulation using our model.

Mechanism of interactions of dsDNA binding with quercetin and its two novel sulfonate derivatives using multispectroscopic, voltammetric, and molecular docking studies

Flavonoids have an important place in chemistry and pharmacology. Several flavonoids, especially Quercetin, have the potential to form molecular complexes with nucleic acid structure and have recently attracted attention due to their prospective clinical and pharmacological uses. DNA is the main target for a wide variety of therapeutic agents. Therefore, there is great interest in studies of binding small molecules with DNA. The interaction of small molecules with DNA provides a structural guide in rational drug design and the synthesis of new and improved drugs with enhanced selective activity and higher clinical efficacy. Even if newly synthesized candidate drug molecules with small molecular weight are capable of indirectly interacting with DNA, the mechanisms that accomplish this need to be clearly known. In this study, the mechanism of fish sperm double strain deoxyribonucleic acid (dsDNA) binding with Quercetin (QCR) and its two novel sulfonate derivatives (quercetin mesylate (QMS) and quercetin tosylate-A (QTS-A)) were researched. For investigating the interaction between the molecules and dsDNA was studied by analytical (spectrophotometric, viscosimetric, and electrochemical) methods. The interaction of dsDNA and two quercetin sulfonate derivatives were compared with the interaction of the QCR standard after all experimental studies. Moreover, the DNA binding constants Kb were determined using each method. The Kb constants calculated for QCR, QMS, and QTS-A are in harmony for all techniques. The results showed that QCR binds to dsDNA via intercalation mode, while QMS and QTS-A bind through minor groove binding mode. In addition to experimental studies, theoretical studies were conducted at room temperature under physiological conditions (pH 7.4). Molecular docking calculations and molecular dynamics (MD) simulations have been found to be compatible with experimental studies.

The role of different inorganic anions on passive film durability for nickel against chloride ions pitting corrosion in borate buffered solution

Abstract Potentiodynamic and cyclic voltammetric studies were carried out on nickel in borate buffered saline (pH = 8.49). The anodic excursion spans of nickel in borate buffer solution do not involve active/passive transition. The passive film starts to break down in the presence of Cl-ions, which causes pitting damage. The data reveal that the increasing Cl− concentration and solution temperature shifts the E pit to the active direction while the increasing in scan rate shifts the E pit to the positive direction. The pitting potential (E pit) shifted in a positive direction when increasing concentrations of Wo4 −2 and MoO4 −2 anions were added to a borate buffer solution containing Cl− ions, showing that the additional anions had an inhibitory influence on the pitting corrosion. While the NO3 − anion is ineffectual as an inhibitor and rather speeds up pitting corrosion, the NO2 − anion has a slight inhibitory impact on pitting corrosion.

Extraction of Np(IV/VI) from nitric acid medium using three different tripodal diglycolamide ligands in ionic liquid: Batch extraction, spectroscopic and electrochemical investigations

Complexation of Np(IV) and Np(VI) ions was studied in a room temperature ionic liquid (C4mim.NTf2) using three tripodal ligands with an ‘N’ atom, a ‘C’ atom and a benzene ring at the center, which are termed as LI, LII and LIII, respectively . The studies include solvent extraction, visible-near infrared (vis-NIR) spectroscopy, and cyclic voltammetry. The trend of the extraction of Np4+ was LIII > LII > LI, which resembled that reported before in a mixture of molecular diluents but with about 10 times higher ligand concentration. Np(VI) was extracted to a much lower extent than Np(IV). Slope analysis of Np(IV) extraction suggested formation of Np(NO3)4.L species for LII and LIII, while a cationic species of the type [Np(NO3)2.L]2+ was seen for LI. On the other hand, for Np(VI), formation of NpO2(NO3)2.L species was proposed for LI and LIII and [NpO2(NO3).L]+ for LII. All the extracted species conform to a ‘solvation’ type extraction except for Np(IV) with LI and Np(VI) with LII which point to a ‘cation-exchange’ mechanism. The complexation of the metal ions with the tripodal ligands was supported by peak shifts in the vis-NIR as well as the cyclic voltammetric studies.

Cr doped CeO2 nanoparticles as supercapacitor electrodes

The consumption of electrical energy has greatly increased lately, and the requirement of portable charge storage devices has also increased. To fulfill this, a versatile rare earth element CeO2 in nanoparticle form is selected and synthesized through a cost effective precipitation method for supercapacitor application. To improve its efficiency, 2% and 4% of transition metal chromium were doped into the ceria lattice, and their electrochemical properties were studied. The cubic fluorite structure with an average crystallite size of all the samples was 16 nm, which was confirmed through x-ray diffraction analysis. Peculiar rice shaped clusters are observed for 2% Cr doped samples through field emission scanning electron microscopy analysis. The N2 adsorption desorption studies were performed to calculate the surface area of the prepared samples. A maximum specific capacitance of 42.6 F g−1 was obtained for the 2% Cr doped CeO2 sample at 5 mV s−1 in 2M KOH in cyclic voltammetric studies. The galvanostatic charge–discharge and electrochemical impedance spectroscopy measurements were also taken to analyze the charge–discharge cycles and stability of the samples.

Sequestration of Np4+ and NpO22+ ions by using diglycolamide-functionalized azacrown ethers in C8mim·NTf2 ionic liquid: Extraction, spectroscopic, electrochemical and DFT studies

Complexation of Np4+ and NpO22+ ions was studied in a room temperature ionic liquid (C8mim•NTf2) using two multiple diglycolamide (DGA) ligands with three and four DGA arms tethered to the nitrogen atoms of the aza-9-crown-3 and -12-crown-4 scaffolds termed as LI and LII, respectively. The studies include solvent extraction, UV–visible spectrophotometry, cyclic voltammetry, and density functional theory (DFT). While the extraction of NpO22+ ion, as a function of the nitric acid concentration, resembled that of the ‘solvation’ mechanism, seen in case of neutral donor ligands in molecular diluent, an opposite trend was observed for the Np4+ ion suggesting a ‘cation-exchange’ mechanism often operating in the case of ionic liquid-based solvent systems. Slope analysis suggested formation of Np(NO3)]3+•L and NpO2(NO3)2•L extracted species for the extraction of Np4+ and NpO22+, respectively, in both the ligand systems. The complexation of the metal ions was supported by peak shifts in the UV–visible spectrophotometric as well as cyclic voltammetric studies. DFT studies were carried out to get structural information of the complexes.

Electropolymerized methylene blue on graphene oxide framework for the direct voltammetric detection of gallic acid

Electropolymerized materials are cost efficient, sensitive and durable for sensor applications. Herein, the cationic dye, methylene blue, electropolymerized on graphene oxide framework using cyclic voltammetry and processed for voltammetric sensor platform. The surface chemistry, topology and wettability of the prepared electrode material was comprehensively studied with Raman spectroscopy, field-emission scanning electron/atomic force microscopes and contact angle measurement. The electrochemical quartz crystal microbalance analysis was done to quantify the mass adsorbed on the graphene oxide framework. Cyclic voltammetric study of the prepared methylene blue-graphene oxide framework electrode exhibits a reversible redox behavior at the electrode-electrolyte interface, following surface confined process with a coefficient determination of 0.99. Electrochemical sensing ability of the prepared electrode material was tested against the clinically important phytomedicine, gallic acid. Linear sweep voltammetric analysis enabled that methylene blue-graphene oxide framework is highly sensitive and selective toward electrooxidation of gallic acid, exerting a detection limit of 49.2 μM in the studied experimental concentration range from 50 μM to 1 mM. Real sample validation with commercial herbal tablet extracts of Euphorbia prostrata containing spiked gallic acid suggest that the prepared sensor platform could be a potential analytical probe for herbaceutical testing.

Voltammetric determination of Molnupiravir used in treatment of the COVID-19 at magnetite nanoparticle modified carbon paste electrode

To reduce the progression of the viral process in patients infected with COVID-19, new treatments and drug active substances are needed. One of these drugs is Molnupiravir (MNP) which has a direct antiviral effect and has also proven to be highly effective in reducing the azopharyngeal SARS-CoV-2 infectious virus and viral RNA. Due to the importance and frequent use of this drug in the treatment of COVID-19, its accurate, quick, and cheap detection in pharmaceutical or biological samples is crucial. In this work, electrochemical behavior and sensitive voltammetric determination of MNP are described using a magnetite nanoparticle modified carbon paste electrode (Fe3O4@CPE) for the first time. Fe3O4 nanoparticles (NPs) were characterized by recording their transmission electron microscopy (TEM) images, energy dispersive X-ray (EDX), and X-ray diffraction (XRD) spectra. Cyclic voltammetric measurements showed that MNP was irreversibly oxidized at Fe3O4@CPE at 760 mV in pH 2.0 Britton Robinson buffer solution (BRBS). The peak current of MNP was increased approximately threefold at Fe3O4@CPE compared to bare CPE due to a good electrocatalytic efficiency of Fe3O4 NPs. According to differential pulse voltammetric studies, the fabricated electrode exhibited a linear range (LR) between 0.25 and 750 µM with sensitivity and limit of detection (LOD) of 4591.0 µA mM−1 cm−2 and 0.05 µM, respectively. On the other hand, although lower sensitivity (327.3 µA mM−1 cm−2) was obtained from CV compared to DPV, a wider linear calibration curve between 0.25 and 1500 µM was obtained in CV. Studies performed in tablet samples confirmed that the Fe3O4@CPE exhibits high applicability for selective and accurate voltammetric determination of MNP in real samples.

Voltammetric studies of the interaction of genotoxic 2-nitrofluorene with DNA

The interaction of genotoxic environmental pollutant 2-nitrofluorene (2-NF) with double-stranded DNA has been studied using a hanging mercury drop electrode (HMDE) as an electrochemical sensor. Two types of DNA damage were investigated and electrochemically detected using cyclic voltammetry and differential pulse voltammetry: (i) DNA damage caused by the direct interaction with 2-NF and (ii) DNA damage caused by short-lived radicals generated by the electrochemical reduction of 2-NF. For the study of the direct interaction, the HMDE was modified by DNA and the interaction of DNA with 2-NF was studied after their mutual interaction right at the HMDE surface, or DNA was preincubated with 2-NF in solution and, subsequently, the interaction was studied voltammetrically. Using both detection techniques, the formation of DNA–2-NF complex was observed and the mutual interaction was interpreted as an intercalation between DNA base pairs. On the basis of obtained results, we suppose that expected formation of 8-oxoguanosine leads to guanosine–cytidine base pair interruption and DNA double-strand break formation. The binding constants (K) of the DNA–2-NF complex formed in solution and on the HMDE surface (DNA/HMDE) were determined from the changes in the voltammetric peaks of the studied analyte.

Surface-engineering of carbon fibre paper electrode through molecular imprinting technique towards electrochemical sensing of food additive in shrimps

Excessive usage of food additives needs to be extensively examined and regulated. Herein, we report the development of an exceptionally proficient and practical electrochemical sensor for the quantitative determination of 4-hexylresorcinol (4-HR) in shrimps using a molecularly imprinted conducting polymer. By electropolymerizing 2-aminothiazole (AT) on the surface of a carbon fibre paper electrode (CFP) in the presence of 4-HR imprinted polymer films were developed. Bulk-electrolysis was used to produce definite imprinting sites and regulate the release of 4-hexylresorcinol templates. Voltammetric study reveals that the synthesized conducting polymer has outstanding electroactivity towards 4-HR and enables quick electron transfer kinetics. This MIP sensor has a detection limit of 6.03 nM for 4-HR. The modified CFP electrode has been found to be extremely selective to 4-HR due to its intensive contact via intermolecular hydrogen bonding. The modified electrodes were characterized by Scanning Electron Microscopy, Fourier Transform Infrared spectroscopy, Optical profilometry, and X-ray Photoelectron Spectroscopy..

Square wave voltammetric study of interaction between 9-acridinyl amino acid derivatives and DNA

Electrochemical oxidation of newly synthesized acridine derivatives (ADs): PG, PA, EG and EA was studied using square wave voltammetry at a glassy carbon electrode. Oxidation occurs as an irreversible process for all ADs. The ADs interaction with DNA was investigated using multi-layer DNA electrochemical biosensor. The shift of dA peak in positive direction indicated that the type of interaction is most likely an intercalation. PG showed the widest range of concentration capable to interact with DNA (1 × 10−7 M − 2.5 × 10−4 M). Analysing logIcomplexIDNA-IcomplexvslogcAD plots, the binding constants were determined. For the lowest PG concentrations, obtained K value close to 106 M−1 refers to strong binding. The values of K for PA may be classified as medium strength, while EG and EA showed low K values. Our results unequivocally showed that the characteristics of association complexes may vary depending on the concentration of the interacting substance. The negative ΔG value for all ADs, (- 21 to - 34 kJ mol−1), confirms the process spontaneity. The best result, indicating the most stable formed complex with DNA adsorbed at the electrode surface, showed PG when present in low concentration, order of 10−7 M. The intercalation of ADs into DNA was supported by molecular docking analysis.

Membrane electrolysis for recovering Sb and Bi from elution solutions of ion-exchange resins used in copper electrorefining: A cyclic voltammetric study

• A membrane electrolysis system was proposed to recover Sb-Bi from HCl solution. • The effects of several parameters on the process were studied by cyclic voltammetry. • The reactions of electrodeposition of Sb-Bi are not electrochemically reversible. • The diffusion control for Bi is greater than for Sb. • The use of thiourea as a complexing agent must be avoided. Antimony (Sb) and bismuth (Bi), which have been considered critical raw materials by the European Commission, cause inconveniences to copper production when they are present as impurities in copper electrorefining solutions. Therefore, ion-exchange resins to extract Sb and Bi from copper-containing electrolytes have typically been applied; after the adsorption of the metals, the elution step is conducted with an HCl solution to desorb them. In the present study, a novel membrane electrolysis system with a cation-exchange membrane was proposed to extract Sb and Bi ions from the elution solution, and a cyclic voltammetric study was carried out to evaluate the influence of the most important operating parameters on the process performance, such as Sb, Bi and HCl concentration, dilution factor of the solution, the presence of thiourea as a complexing agent, the presence of iron as an impurity, and temperature. The obtained voltammograms indicated that the simultaneous presence of the metals in solution alters considerably their electrodeposition and oxidation pattern when compared to the solutions with pure metals. The reactions of electrodeposition of both metals are not electrochemically reversible and the diffusion control for bismuth is greater than that for antimony. The increase in the concentration of Sb affects its electrodeposition kinetically, whereas that of Bi is affected both kinetically and thermodynamically. The increase in HCl concentration disfavors the electrodeposition of both metals. Diluting the solution reduces the energy consumption and prolongs the membrane lifespan. Increasing the temperature reduces the cathodic potential to deposit the metals but favors the hydrogen evolution reaction. The presence of iron as an impurity does not affect the electrodeposition of both metals, whereas the use of thiourea as a complexing agent must be avoided because it impairs their electrodeposition.