Search Results (63)

Recently, it has been found that electrochemical sensing technology is one of the significant approaches for the monitoring of toxic and hazardous substances in food and the environment. Nitrofurazone (NFZ) and nitrofurantoin (NFT) possess a hazardous influence on the environment, aquatic life, and human health. Thus, various advanced materials such as graphene, carbon nanotubes, metal oxides, MXenes, layered double hydroxides (LDHs), polymers, metal–organic frameworks (MOFs), metal-based composites, etc. are widely used for the development of nitrofurazone and nitrofurantoin sensors. This review article summarizes the progress in the fabrication of electrode materials for nitrofurazone and nitrofurantoin sensing applications. The performance of the various electrode materials for nitrofurazone and nitrofurantoin monitoring are discussed. Various electrochemical sensing techniques such as square wave voltammetry (SWV), differential pulse voltammetry (DPV), linear sweep voltammetry (LSV), amperometry (AMP), cyclic voltammetry (CV), and chronoamperometry (CA) are discussed for the determination of NFZ and NFT. It is observed that DPV, SWV, and AMP/CA are more sensitive techniques compared to LSV and CV. The challenges, future perspectives, and limitations of NFZ and NFT sensors are also discussed. It is believed that present article may be useful for electrochemists as well materials scientists who are working to design electrode materials for electrochemical sensing applications. Full article

The utilization of geothermal resources as renewable energy is a subject of interest for the regions that possess these resources. The exploitation of geothermal energy must consider local geological conditions and an integrated approach, which should include practical studies on the chemistry of geothermal waters and their effect on thermal installations. Geothermal waters from Bihor County, Romania, have a variable composition, depending on the crossed geological layers, but also on pressure and temperature. Obviously, water transport and heat transfer are involved in all applications of geothermal waters. This article aims to characterize certain geothermal waters from the point of view of composition and corrosion if used as a thermal agent. Atomic absorption spectroscopy (AAS) and UV–Vis spectroscopy were employed to analyze water specimens. Chemical composition includes calcite (CaCO₃), chalcedony (SiO₂), goethite (FeO(OH)), and magnetite (Fe₃O₄), which confirms the corrosion and scale potential of these waters. Corrosion resistance of mild carbon steel, commonly used as pipe material, was studied by the gravimetric method and through electrochemical methodologies, including chronoamperometry, electrochemical impedance spectroscopy (EIS), potentiodynamic polarization method, and open circuit potential measurement (OCP). Statistical analysis shows that the medium corrosion rate of S235 steel, expressed as penetration rate, is between 0.136 mm/year to 0.615 mm/year. The OCP, EIS, and chronoamperometry experiments explain corrosion resistance through the formation of a passive layer on the surface of the metal. This study proposes an innovative methodology and a systematic algorithm for analyzing chemical processes and corrosion phenomena in geothermal installations, emphasizing the necessity of individualized assessments for each aquifer to optimize operational parameters and ensure sustainable resource utilization. Full article

This study aims to develop and validate a novel fast-detection electrochemical sensing platform to enhance portable electrochemical sensor solutions. The research focuses on optimising analogue front-end circuits, developing data analysis algorithms, and validating the device through experiments to enhance measurement accuracy and detection speed, enabling on-site measurements across diverse applications. This work successfully designed a Portable Unit for Lab-on-Site Electrochemistry (PULSE) system with dimensions of $(78\times 100\times 2)$ ${\mathrm{mm}}^3$. The device’s implementation was complemented by robust firmware that performed desired electrochemical measurements, including open circuit potentiometry (OCP), chronoamperometry (CA), and cyclic voltammetry (CV). To assess its reliability, the PULSE was benchmarked against a well-established benchtop potentiostat. The results obtained highlight the system’s rapid sensing capabilities, achieving pH detection in 2 s and performing CA in 20 s. The pH calibration curve exhibited Nernstian behaviour with an accuracy of 97.58%. A correlation analysis comparing the calibration curve datasets across all electrochemical techniques from both systems revealed high correlation coefficients (>0.99), confirming the strong agreement between the two systems. Full article

This study presents the findings of an investigation into the characteristics and capabilities of BiVO₄ and Mo-doped BiVO₄ coatings for the detection of diclofenac (DCF). In this study, a neutral sodium sulfate electrolyte and an alkaline sodium borate buffer were selected, and a range of potentials were employed to ascertain the impact of diverse conditions on the sensing performance of diclofenac. The introduction of Mo-doping had a profound impact on the photoelectrochemical response of the BiVO₄ coating. However, it was observed that Mo-doping resulted in an increase in the adsorption of diclofenac oxidation products on the surface of the photoanode, which in turn led to a negative blocking effect. To evaluate the structural and morphological properties of the coatings, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and energy dispersive analysis (EDX) were conducted. The photoelectrochemical properties were evaluated through the use of cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and chronoamperometry (CA). An increase in the photocurrent density of BiVO₄ was observed in response to an increase in the concentration of diclofenac within a range of 0.1 to 1 mg L⁻¹ during the sensing experiments. However, at higher concentrations, saturation of diclofenac was observed at the photoelectrode/electrolyte interface. The results of selectivity experiments demonstrated that the nature of the electrolyte has a significant impact on the selectivity of designed photoelectrochemical sensors. Full article

For the first time, nitrogen- and carbon-present tin dioxide-supported palladium composite catalysts (denoted as Pd/N-C-SnO₂) were prepared via an HCH method (HCH is the abbreviation for the hydrothermal process–calcination–hydrothermal process preparation process). In this work, firstly, three catalyst carriers (denoted as cc) were prepared using a hydrothermal-process-aided calcination method, and catalyst carriers prepared using ammonia monohydrate (NH₃∙H₂O), N,N-dimethylformamide (C₃H₇NO) and triethanolamine (C₆H₁₅NO₃) as the nitrogen sources were nominated as cc₁, cc₂ and cc₃, respectively. Secondly, these catalyst carriers were reacted with palladium oxide monohydrate (PdO·H₂O) hydrothermally to generate catalysts c₁, c₂ and c₃. As testified by XRD and XPS, besides carbon materials and the N-containing substances, the main substances of all prepared catalysts were SnO₂ and metallic palladium (Pd). Above all things, all resultant catalysts, especially c₂, showed a prominent electrocatalytic activity towards the ethanol oxidation reaction (EOR). As indicated by the CV (cyclic voltammetry) results, all fabricated catalysts presented a clear electrocatalytic activity towards the EOR. In the CA (chronoamperometry) measurement, the faradaic current density of EOR measured on c₂ at −0.27 V vs. an SCE (saturated calomel electrode) after 7200 s was still maintained at about 5.6 mA cm⁻². Preparing a novel catalyst carrier, N-C-SnO₂, and preparing a new EOR catalyst, Pd/N-C-SnO₂, were the principal dedications of this preliminary work, which was very beneficial to the development of Pd-based EOR catalysts. Full article

Cerium dioxide (CeO₂) is a promising material for photoelectrochemical applications, requiring a thorough understanding of the interplay between its properties and structure for optimal performance. This study investigated the photoelectrochemical performance of CeO₂ photoanodes immobilized by electrodeposition on glass substrates, focusing on the correlation between the annealing temperature and structural, optical, and electrical changes. CeO₂ coatings were obtained via chronoamperometry in an aqueous solution of 25 mM CeCl₃ and 50 mM NaNO₃. The photoelectrochemical characterization included the evaluation of photoactivity, current density, stability, and recombination using linear sweep voltammetry (LSV) and chronoamperometry (CA). Charge transfer resistance, flat-band potential, and capacitance were assessed through impedance spectroscopy. The optimal annealing temperature for this material was found to be 600 °C as it resulted in the lowest charge transfer resistance and increased photocurrent, which was attributed to enhanced crystallinity and variations in the Ce³⁺/Ce⁴⁺ ratio. Full article

In this research, a novel electrochemical biosensor is proposed based on inducing graphene formation on polyimide substrate via laser engraving. Graphene polyaniline (G-PANI) conductive ink was synthesized by planetary mixing and applied to the working zone of the developed sensor to effectively enhance the electrical signals. The laser-induced graphene (LIG) sensor was used to detect alpha-fetoprotein (AFP) and 17β-Estradiol (E2) in the phosphate buffer saline (PBS) buffer and human serum. The electrochemical performance of the biosensor in determining these biomarkers was investigated by differential pulse voltammetry (DPV) and chronoamperometry (CA). In a buffer environment, alpha-fetoprotein (AFP) and 17β-Estradiol detection range were 4–400 ng/mL and 20–400 pg/mL respectively. The experimental results showed a limit of detection (LOD) of 1.15 ng/mL and 0.96 pg/mL for AFP and estrogen, respectively, with an excellent linear range (R² = 0.98 and 0.99). In addition, the designed sensor was able to detect these two types of biomarkers in human serum successfully. The proposed sensor exhibited excellent reproducibility, repeatability, and good stability (relative standard deviation, RSD = 0.96%, 1.12%, 2.92%, respectively). The electrochemical biosensor proposed herein is easy to prepare and can be successfully used for low-cost, rapid detection of AFP and E2. This approach provides a promising platform for clinical detection and is advantageous to healthcare applications. Full article

The enhancement of carbon-supported components is a crucial factor in augmenting the interplay between carbon-supported and metal-active components in the utilization of catalysts for direct ethanol fuel cells (DEFCs). Here, we propose a strategy for designing a catalyst by modifying candle soot (CS) and loading nickel onto ordered carbon soot. The present study aimed to investigate the effect of the Ni nanoparticles content on the electrocatalytic performance of Ni–CS, ultimately leading to the identification of a maximum composition. The presence of an excessive quantity of nickel particles leads to a decrease in the number of active sites within the material, resulting in sluggishness of the electron transfer pathway. The electrocatalyst composed of nickel and carbon support, with a nickel content of 20 wt%, has demonstrated a noteworthy current activity of 18.43 mA/cm², which is three times that of the electrocatalyst with a higher nickel content of 25 wt%. For example, the 20 wt% Ni–CS electrocatalytic activity was found to be good, and it was approximately four times higher than that of 20 wt% Ni–CB (nickel–carbon black). Moreover, the chronoamperometry (CA) test demonstrated a reduction in current activity of merely 65.80% for a 20 wt% Ni–CS electrocatalyst, indicating electrochemical stability. In addition, this demonstrates the great potential of candle soot with Ni nanoparticles to be used as a catalyst in practical applications. Full article

Preparing high-performance oxygen evolution reaction (OER) catalysts with low precious metal loadings for water electrolysis applications (e.g., for green hydrogen production) is challenging and requires electrically conductive, high-surface-area, and stable support materials. Combining the properties of stable TiO₂ with those of active iridium oxide, we synthesized highly active electrodes for OER in acidic media. TiO₂ powders (both commercially available Degussa P-25^® and hydrothermally prepared in the laboratory from TiOSO₄, either as received/prepared or following ammonolysis to be converted to titania black), were decorated with IrO₂ by UV photodeposition from Ir(III) aqueous solutions of varied methanol scavenger concentrations. TEM, EDS, FESEM, XPS, and XRD measurements demonstrate that the optimized version of the photodeposition preparation method (i.e., with no added methanol) leads to direct deposition of well-dispersed IrO₂ nanoparticles. The electroactive surface area and electrocatalytic performance towards OER of these catalysts have been evaluated by cyclic voltammetry (CV), Linear Sweep Voltammetry (LSV), and Electrochemical Impedance Spectroscopy (EIS) in 0.1 M HClO₄ solutions. All TiO₂-based catalysts exhibited better mass-specific (as well as intrinsic) OER activity than commercial unsupported IrO₂, with the best of them (IrO₂ on Degussa P-25^® ΤiO₂ and laboratory-made TiO₂ black) showing 100 mAmg_Ir⁻¹ at an overpotential of η = 243 mV. Chronoamperometry (CA) experiments also proved good medium-term stability of the optimum IrO₂/TiO₂ electrodes during OER. Full article

This study examines the catalytic activity of NiFeCoO_x catalysts for anion exchange membrane (AEM) water electrolysis. The catalysts were synthesized with a Ni to Co ratio of 2:1 and Fe content ranges from 2.5 to 12.5 wt%. The catalysts were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. The catalytic activity of the NiFeCoO_x catalysts was evaluated through linear sweep voltammetry (LSV) and chronoamperometry (CA) experiments for the oxygen evolution reaction (OER). The catalyst with 5% Fe content exhibited the highest catalytic activity, achieving an overpotential of 228 mV at a current density of 10 mA cm⁻². Long-term catalyst testing for the OER at 50 mA cm⁻² showed stable electrolysis operation for 100 h. The catalyst was further analyzed in an AEM water electrolyzer in a single-cell test, and the NiFeCoO_x catalyst with 5% Fe at the anode demonstrated the highest current densities of 1516 mA cm⁻² and 1620 mA cm⁻² at 55 °C and 70 °C at 2.1 V. The maximum current density of 1880 mA cm⁻² was achieved at 2.2 V and 70 °C. The Nyquist plot analysis of electrolysis at 55 °C showed that the NiFeCoO_x catalyst with 5% Fe had lower activation resistance compared with the other Fe loadings, indicating enhanced performance. The durability test was performed for 8 h, showing stable AEM water electrolysis with minimum degradation. An overall cell efficiency of 70.5% was achieved for the operation carried out at a higher current density of 0.8 A cm⁻². Full article

Polymer electrolyte was used as a medium for testing the performance of microband electrodes under conditions of linear diffusion. Cyclic voltammetry (CV) and chronoamperometry (CA) experiments were performed in a highly viscous medium, where diffusion rates are much slower than in fluid solutions. The log i vs. log v (CV) or log i vs. log t (CA) relationships with the current equation confirmed the existence of such conditions, yielding slope values that were lower than the expected 0.5. This could indicate an impure linear diffusion profile, i.e., some contribution from radial diffusion (edge effects). However, the desired value of 0.5 was obtained when performing these tests in monomeric solvents of similar viscosities, such as glycerol or propylene glycol. These results led to the conclusion that the current equations, which are based on Fick’s laws, may not be applicable for polymer electrolytes, where various obstructions to free diffusion result in a more complicated process than for monomeric solvents. Full article

The design of efficient oxygen evolution reaction (OER) electrocatalysts is of great significance for improving the energy efficiency of water electrolysis for hydrogen production. In this work, low-temperature fluorination and the introduction of a conductive substrate strategy greatly improve the OER performance in alkaline solutions. Cobalt–iron fluoride nanosheets supported on reduced graphene architectures are constructed by a one-step solvothermal method and further low-temperature fluorination treatment. The conductive graphene architectures can increase the conductivity of catalysts, and the transition metal ions act as electron acceptors to reduce the Fermi level of graphene, resulting in a low OER overpotential. The surface of the catalyst becomes porous and rough after fluorination, which can expose more active sites and improve the OER performance. Finally, the catalyst exhibits excellent catalytic performance in 1 M KOH, and the overpotential is 245 mV with a Tafel slope of 90 mV dec⁻¹, which is better than the commercially available IrO₂ catalyst. The good stability of the catalyst is confirmed with a chronoamperometry (CA) test and the change in surface chemistry is elucidated by comparing the XPS before and after the CA test. This work provides a new strategy to construct transition metal fluoride-based materials for boosted OER catalysts. Full article

This work reports the influence of a reduced graphene oxide (rGO) support on the catalytic performance of Cu@PtRu/rGO electrocatalysts toward methanol oxidation in an acidic medium. These electrocatalysts are synthesized via a two-step reduction method; the first step utilizes ethylene glycol for the reduction of Cu²⁺ ions, forming Cu/rGO. In the second step, spontaneous redox reactions take place, in a process known as galvanic displacement, where the Pt²⁺ and Ru³⁺ species are reduced to form PtRu layers, and the copper is partially oxidized to the solution. Then, the Cu@PtRu/rGO core–shell is produced, comprising Cu in the inner structure (core) and PtRu on the outer part (shell). To compare the catalytic performance of the prepared nanocatalysts (NCs), Pt/C, PtRu/C, and Cu@PtRu/C are also synthesized on Vulcan XC-72R carbon. All catalysts are characterized via X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Cyclic voltammetry (CV) and chronoamperometry (CA) are employed to measure the electrochemical performance. The core–shell/rGO combination is superior in catalytic activity to the traditional Pt/C, PtRu/C, and Cu@PtRu/C catalysts for the methanol oxidation reaction. These results suggest that Cu@PtRu/rGO exhibits a high bulk activity for methanol electrooxidation, a high stability, and a high tolerance to CO poisoning, meaning it is possible to reduce the platinum loading in proton-exchange membrane fuel cells (PEMFCs). Full article

Herein, a simple method has been used in the fabrication of a microneedle electrode (MNE). To do this, firstly, a commercial self-dissolving microneedle patch has been used to make a hard-polydimethylsiloxane-based micro-pore mold (MPM). Then, the pores of the MPM were filled with the conductive platinum (Pt) paste and cured in an oven. Afterward, the MNE made of platinum (Pt-MNE) was characterized using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and scanning electron microscopy (SEM). To prove the electrochemical applicability of the Pt-MNE, the glutamate oxidase enzyme was immobilized on the surface of the electrode, to detect glutamate, using the cyclic voltammetry (CV) and chronoamperometry (CA) methods. The obtained results demonstrated that the fabricated biosensor could detect a glutamate concentration in the range of 10–150 µM. The limits of detection (LODs) (three standard deviations of the blank/slope) were also calculated to be 0.25 µM and 0.41 µM, using CV and CA, respectively. Furthermore, the Michaelis–Menten constant (K_M^app) of the biosensor was calculated to be 296.48 µM using a CA method. The proposed biosensor was finally applied, to detect the glutamate concentration in human serum samples. The presented method for the fabrication of the mold signifies a step further toward the fabrication of a microneedle electrode. Full article

Thin layers (up to 1 µm) of Pd-Ir alloys were electrodeposited from aqueous, galvanic baths of PdCl₂ and IrCl₃ mixtures. The morphology of the electrodeposits was examined by means of scanning electron microscopy. The composition of alloys was determined with the use of energy-dispersive spectroscopy, atomic absorption spectrometry, X-ray photoelectron spectroscopy, and Auger electron spectroscopy. For the studies of the electrochemical properties of alloys, cyclic voltammetry, chronoamperometry, and chronopotentiometry were used. It was found that Pd-Ir alloy electrodes were surface-enriched with Pd. Pd-Ir alloys subjected to different electrochemical treatment involving hydrogen sorption changed their surface state. The continuous hydrogen sorption enhanced the Ir ions’ dissolution. The values of thermodynamic functions of hydrogen sorption in strong alkaline electrolytes were comparable with those in acidic electrolytes, whereas the kinetics of the process in alkaline medium was hindered. The miscibility gap in the Pd-Ir-H system vanished for the electrode containing ca. 93.7 at.% Pd. Full article