Search results for: Voltammetry

Authors: Mandlenkosi George Robert Mahlobo, Peter Apata Olubambi, Philippe Refait

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The aim of this study was to use voltammetry as a method to understand the behavior of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP which was only applied on two of the three coupons at the protection potential -0.8 V vs. Cu/CuSO4 for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from ohmic drop. Voltammetry was finally performed the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduce the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect, from the decreased potential, and an induced effect, associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: Carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy.

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Authors: Y. El Kaissi, M. Allam, A. Koulou, M. Galai, M. Ebn Touhami

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The aim of our work is to develop an industrial bath of nickel alloy deposit on mild steel. The optimization of the operating parameters made it possible to obtain a stable Ni-P alloy deposition formulation. To understand the reaction mechanism of the deposition process, a kinetic study was performed by cyclic voltammetry and by electrochemical impedance spectroscopy (EIS). The coatings obtained have a very high corrosion resistance in a very aggressive acid medium which increases with the heat treatment.

Keywords: Ni–P coating, electrochemical impedance spectroscopy, heat treatment, cyclic voltammetry, potentiodynamic polarization.

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Authors: Alexey P. Antropov, Alexander V. Ragutkin, Nicolay A. Yashtulov

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The original controlled technology for power active nanocomposite membrane-electrode assembly engineering on the basis of porous silicon is presented. The functional nanocomposites were studied by electron microscopy and cyclic voltammetry methods. The application possibility of the obtained nanocomposites as high performance renewable energy sources for micro-power electronic devices is demonstrated.

Keywords: Cyclic voltammetry, electron microscopy, nanotechnology, platinum-palladium nanocomposites, porous silicon, power activity, renewable energy sources.

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Authors: Amer Dawoud, Rashid Mia, Arati Biswakarma, Jesy Motchaalangaram, Wujan Miao, Karl Wallace

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The development of an embedded miniaturized drone-based system for remote detection of Chemical Warfare Agents (CWAs) is proposed. The paper focuses on the software/hardware system design of the electrochemical Cyclic Voltammetry (CV) and Differential Pulse Voltammetry (DPV) signal processing for future deployment on drones. The paper summarizes the progress made towards hardware and electrochemical signal processing for signature detection of CWA. Also, the miniature potentiostat signal is validated by comparing it with the high-end lab potentiostat signal.

Keywords: Drone-based, remote detection chemical warfare agents, miniaturized, potentiostat.

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Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

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Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750oC analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: Carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry.

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Authors: Soroor Ghaziof, Wei Gao

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Zn alloy and composite coatings are widely used in buildings and structures, automobile and fasteners industries to protect steel component from corrosion. In this paper, Zn-Ni-Al2O3 nanocomposite coatings were electrodeposited on mild steel using a novel sol enhanced electroplating method. In this method, transparent Al2O3 sol was added into the acidic Zn-Ni bath to produced Zn-Ni- Al2O3 nanocomposite coatings. The effect of alumina sol on the electrodeposition process, and coating properties was investigated using cyclic voltammetry, XRD, ESEM and Tafel test. Results from XRD tests showed that the structure of all coatings was single γ- Ni5Zn21 phase. Cyclic voltammetry results showed that the electrodeposition overpotential was lower in the presence of alumina sol in the bath, and caused the reduction potential of Zn-Ni to shift to more positive values. Zn-Ni-Al2O3 nanocomposite coatings produced more uniform and compact deposits, with fine grained microstructure when compared to Zn-Ni coatings. The corrosion resistance of Zn-Ni coatings was improved significantly by incorporation of alumina nanoparticles into the coatings.

Keywords: Zn-Ni-Al2O3 composite coatings, steel, sol-enhanced electroplating, corrosion resistance.

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Authors: M. Ardelean, F. Manea, A. Pop, J. Schoonman

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The presence of pharmaceuticals in the environment and especially in water has gained increasing attention. They are included in emerging class of pollutants, and for most of them, legal limits have not been set-up due to their impact on human health and ecosystem was not determined and/or there is not the advanced analytical method for their quantification. In this context, the development of various advanced analytical methods for the quantification of pharmaceuticals in water is required. The electrochemical methods are known to exhibit the great potential for high-performance analytical methods but their performance is in direct relation to the electrode material and the operating techniques. In this study, two types of carbon-based electrodes materials, i.e., boron-doped diamond (BDD) and carbon nanofiber (CNF)-epoxy composite electrodes have been investigated through voltammetric techniques for the detection of naproxen in water. The comparative electrochemical behavior of naproxen (NPX) on both BDD and CNF electrodes was studied by cyclic voltammetry, and the well-defined peak corresponding to NPX oxidation was found for each electrode. NPX oxidation occurred on BDD electrode at the potential value of about +1.4 V/SCE (saturated calomel electrode) and at about +1.2 V/SCE for CNF electrode. The sensitivities for NPX detection were similar for both carbon-based electrode and thus, CNF electrode exhibited superiority in relation to the detection potential. Differential-pulsed voltammetry (DPV) and square-wave voltammetry (SWV) techniques were exploited to improve the electroanalytical performance for the NPX detection, and the best results related to the sensitivity of 9.959 µA·µM^-1 were achieved using DPV. In addition, the simultaneous detection of NPX and fluoxetine -a very common antidepressive drug, also present in water, was studied using CNF electrode and very good results were obtained. The detection potential values that allowed a good separation of the detection signals together with the good sensitivities were appropriate for the simultaneous detection of both tested pharmaceuticals. These results reclaim CNF electrode as a valuable tool for the individual/simultaneous detection of pharmaceuticals in water.

Keywords: Boron-doped diamond electrode, carbon nanofiber-epoxy composite electrode, emerging pollutants, pharmaceuticals.

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Authors: Imene Atek, Abed M. Affoune, Hubert Girault, Pekka Peljo

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Due to the need for a rigorous mathematical model that can help to estimate kinetic properties for soluble-insoluble systems, through voltammetric experiments, a Nicholson Semi Analytical Approach was used in this work for modeling and prediction of theoretical linear sweep voltammetry responses for reversible, quasi reversible or irreversible electron transfer reactions. The redox system of interest is a one-step metal electrodeposition process. A rigorous analysis of simulated linear scan voltammetric responses following variation of dimensionless factors, the rate constant and charge transfer coefficients in a broad range was studied and presented in the form of the so called kinetic zones diagrams. These kinetic diagrams were divided into three kinetics zones. Interpreting these zones leads to empirical mathematical models which can allow the experimenter to determine electrodeposition reactions kinetics whatever the degree of reversibility. The validity of the obtained results was tested and an excellent experiment–theory agreement has been showed.

Keywords: Electrodeposition, kinetics diagrams, modeling, voltammetry.

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Authors: Soukaina Motia, Nadia El Alami El Hassani, Alassane Diouf, Benachir Bouchikhi, Nezha El Bari

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Parabens are the antimicrobial molecules largely used in cosmetic products as a preservative agent. Among them, the methylparaben (MP) is the most frequently used ingredient in cosmetic preparations. Nevertheless, their potential dangers led to the development of sensible and reliable methods for their determination in environmental samples. Firstly, a sensitive and selective molecular imprinted polymer (MIP) based on screen-printed gold electrode (Au-SPE), assembled on a polymeric layer of carboxylated poly(vinyl-chloride) (PVC-COOH), was developed. After the template removal, the obtained material was able to rebind MP and discriminate it among other interfering species such as glucose, sucrose, and citric acid. The behavior of molecular imprinted sensor was characterized by Cyclic Voltammetry (CV), Differential Pulse Voltammetry (DPV) and Electrochemical Impedance Spectroscopy (EIS) techniques. Then, the biosensor was found to have a linear detection range from 0.1 pg.mL^-1 to 1 ng.mL^-1 and a low limit of detection of 0.12 fg.mL^-1 and 5.18 pg.mL^-1 by DPV and EIS, respectively. For applications, this biosensor was employed to determine MP content in four wastewaters in Meknes city and two cosmetic products (shower gel and shampoo). The operational reproducibility and stability of this biosensor were also studied. Secondly, another MIP biosensor based on tungsten trioxide (WO₃) functionalized by gold nanoparticles (Au-NPs) assembled on a polymeric layer of PVC-COOH was developed. The main goal was to increase the sensitivity of the biosensor. The developed MIP biosensor was successfully applied for the MP determination in wastewater samples and cosmetic products.

Keywords: Cosmetic products, methylparaben, molecularly imprinted polymer, wastewater.

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Authors: Aniela Pop, Ianina Birsan, Corina Orha, Rodica Pode, Florica Manea

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Carbon nanofiber-epoxy composite electrode has been investigated through voltammetric and amperometric techniques in order to detect parabens from aqueous solutions. The occurrence into environment as emerging pollutants of these preservative compounds has been extensively studied in the last decades, and consequently, a rapid and reliable method for their quantitative quantification is required. In this study, methylparaben (MP) and propylparaben (PP) were chosen as representatives for paraben class. The individual electrochemical detection of each paraben has been successfully performed. Their electrochemical oxidation occurred at the same potential value. Their simultaneous quantification should be assessed electrochemically only as general index of paraben class as a cumulative signal corresponding to both MP and PP from solution. The influence of pH on the electrochemical signal was studied. pH ranged between 1.3 and 9.0 allowed shifting the detection potential value to smaller value, which is very desired for the electroanalysis. Also, the signal is better-defined and higher sensitivity is achieved. Differential-pulsed voltammetry and square-wave voltammetry were exploited under the optimum pH conditions to improve the electroanalytical performance for the paraben detection. Also, the operation conditions were selected, i.e., the step potential, modulation amplitude and the frequency. Chronomaprometry application as the easiest electrochemical detection method led to worse sensitivity, probably due to a possible fouling effect of the electrode surface. The best electroanalytical performance was achieved by pulsed voltammetric technique but the selection of the electrochemical technique is related to the concrete practical application. A good reproducibility of the voltammetric-based method using carbon nanofiber-epoxy composite electrode was determined and no interference effect was found for the cation and anion species that are common in the water matrix. Besides these characteristics, the long life-time of the electrode give to carbon nanofiber-epoxy composite electrode a great potential for practical applications.

Keywords: Carbon nanofiber-epoxy composite electrode, electroanalysis, methylparaben, propylparaben.

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Authors: Wanida Wonsawat

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This research describes a voltammetric approach to determine amounts of vitamin C (Ascorbic acid) in orange juice sample, using three screen printed electrode. The anodic currents of vitamin C were proportional to vitamin C concentration in the range of 0 – 10.0 mM with the limit of detection of 1.36 mM. The method was successfully employed with 2 µL of the working solution dropped on the electrode surface. The proposed method was applied for the analysis of vitamin C in packed orange juice without sample purification or complexion of sample preparation step.

Keywords: Ascorbic acid, Vitamin C, Juice, Voltammetry

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Authors: Mandana Amiri, Sima Nouhi, Yashar Azizan-Kalandaragh

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Silver nanostructures have been successfully fabricated by using electrodeposition method onto indium-tin-oxide (ITO) substrate. Scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and ultraviolet-visible spectroscopy (UV-Vis) techniques were employed for characterization of silver nanostructures. The results show nanostructures with different morphology and electrochemical properties can be obtained by various the deposition potentials and times. Electrochemical behavior of the nanostructures has been studied by using cyclic voltammetry. Silver nanostructures exhibits good electrocatalytic activity towards the reduction of H₂O₂. The presented electrode can be employed as sensing element for hydrogen peroxide.

Keywords: Electrochemical sensor, electrodeposition, hydrogen peroxide, silver nanostructures.

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Authors: Irshad U. Khan, Tanmay Paul, Murali Mohan Seepana

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This paper presents a study on synthesizing and characterizing a Copper Oxide Doped Carbon (CuO-C) electrocatalyst for the negative half-cell reactions of Vanadium Redox Flow Battery (VRFB). The CuO was synthesized using a microreactor. The electrocatalyst was characterized using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Field Emission Scanning Electron Microscopy (SEM). The electrochemical performance was assessed by Linear Sweep Voltammetry (LSV). The findings suggest that the synthesized CuO exhibited favorable crystallinity, morphology, and surface area, leading to improved cell performance.

Keywords: ECSA, electrocatalyst, energy storage, Tafel.

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Authors: N. M. Ahmad, J. Abdullah, N. I. Ramli, S. Abd Rahman, N. E. Azmi, Z. Hamzah, A. Saat, N. H. Rahman

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A biosensor based on glucose oxidase (GOx) immobilized onto nanoparticles zirconium oxide with polyethylene nanocomposite for glucose monitoring has been designed. The CTAB/PEG/ZrO2/GOx nanocomposite was deposited onto screen printed carbon paste (SPCE) electrode via spin coating technique. The properties of CTAB/PEG/ZrO2/GOx were study using scanning electron microscopy (SEM). The SPE modified with the CTAB/PEG/ZrO2/GOx showed electrocatalytical response to the oxidation of glucose when ferrocene carboxaldehyde was used as an artificial redox mediator, which was studied by cyclic voltammetry (CV). Several parameters such as working potential, effect of pH and effect of ZrO2/PEG layers that governed the analytical performance of the biosensor, have been studied. The biosensor was applied to detect glucose with a linear range of 0.4 to 2.0 mmol L−1 with good repetability and reproducibility.

Keywords: Nanocomposite, Nanoparticles, Modified SPE, Ferrocenecarboxaldehyde.

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Authors: Jyoti Narayan, S. Choudhary

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Nanowire arrays of copper with uniform diameters have been synthesized by potentiostatic electrochemical metal deposition (EMD) of copper sulphate and potassium chloride solution within the nano-channels of porous Indium-Tin Oxide (ITO), also known as Tin doped Indium Oxide templates. The nanowires developed were fairly continuous with diameters ranging from 110-140 nm along the entire length. Single as well as poly-crystalline copper wires have been prepared by application of appropriate potential during the EMD process. Scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), small angle electron diffraction (SAED) and atomic force microscopy (AFM) were used to characterize the synthesized nano wires at room temperature. The electrochemical response of synthesized products was evaluated by cyclic voltammetry while surface energy analysis was carried out using a Goniometer.

Keywords: Electro-deposition, Metallic nano-wires, Nanomaterials, Template synthesis

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Authors: Leila Samiee, Amir Yadegari, Saeedeh Tasharrofi

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In the work presented here, nitrogen-doped graphene materials were synthesized and used as metal-free electrocatalysts for oxygen reduction reaction (ORR) under alkaline conditions. Paraphenylenediamine was used as N precursor. The N-doped graphene was synthesized under hydrothermal treatment at 200°C. All the materials have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS). Moreover, for electrochemical evaluation of samples, Rotating Disk electrode (RDE) and Cyclic Voltammetry techniques (CV) were employed. The resulting material exhibits an outstanding catalytic activity for the oxygen reduction reaction (ORR) as well as excellent resistance towards methanol crossover effects, indicating their promising potential as ORR electrocatalysts for alkaline fuel cells.

Keywords: Alkaline fuel cell, graphene, metal-free catalyst, paraphenylenediamine.

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Authors: Kartika S. Hamdan, Zainiharyati M. Zain, Mohamed I. A. Halim, Jafri M. Abdullah, Robert D. O'Neill

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This work attempts to improve the permselectivity of poly-ortho-phenylenediamine (PPD) coating for glutamate biosensor applications on Pt microelectrode, using constant potential amperometry and cyclic voltammetry. Percentage permeability of the modified PPD microelectrode was carried out towards hydrogen peroxide (H2O2) and ascorbic acid (AA) whereas permselectivity represents the percentage interference by AA in H2O2 detection. The 50-μm diameter Pt disk microelectrode showed a good permeability value toward H2O2 (95%) and selectivity against AA (0.01%) compared to other sizes of electrode studied here. The electrode was further modified with glutamate oxidase (GluOx) that was immobilized and cross linked with glutaraldehyde (GA, 0.125%), resulting in Pt/PPD/GluOx-GA electrode design. The maximum current density Jmax and apparent Michaelis constant, KM, obtained on Pt/PPD/GluOx-GA electrodes were 48 μA cm-2 and 50 μM, respectively. The linear region slope (LRS) was 0.96 μA cm-2 mM-1. The detection limit (LOD) for glutamate was 3.0 ± 0.6 μM. This study shows a promising glutamate microbiosensor for brain glutamate detection. 

Keywords: Brain, Glutamate, Microbiosensor.

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Authors: Kashima Arora, Monika Tomar, Vinay Gupta

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Langmuir–Blodgett (LB) films of polyaniline (PANI) grown onto ITO coated glass substrates were utilized for the fabrication of Uric acid biosensor for efficient detection of uric acid by immobilizing Uricase via EDC–NHS coupling. The modified electrodes were characterized by atomic force microscopy (AFM). The response characteristics after immobilization of uricase were studied using cyclic voltammetry and electrochemical impedance spectroscopy techniques. The uricase/PANI/ITO/glass bioelectrode studied by CV and EIS techniques revealed detection of uric acid in a wide range of 0.05 mM to 1.0 mM, covering the physiological range in blood. A low Michaelis–Menten constant (Km) of 0.21 mM indicates the higher affinity of immobilized Uricase towards its analyte (uric acid). The fabricated uric acid biosensor based on PANI LB films exhibits excellent sensitivity of 0.21 mA/mM with a response time of 4 s, good reproducibility, long shelf life (8 weeks) and high selectivity.

Keywords: Uric acid; biosensor, PANI, Langmuir Blodgett films deposition.

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Authors: Chih-Ming Wang, Chih-Yu Wen, Ying-Chung Chen, Chun-Chieh Wang, Chien-Chung Hsu, Jui-Yang Chang, Jyun-Min Lin

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In this study, we developed a complementary electrochromic device consisting of WO₃ and NiO films fabricated by rf-magnetron sputtered. The electrochromic properties of WO₃ and NiO films were investigated using cyclic voltammograms (CV), performed on WO₃ and NiO films immersed in an electrolyte of 1 M LiClO₄ in propylene carbonate (PC). Optical and electrochemical of the films, as a function of coloration–bleaching cycle, were characterized using an UV-Vis-NIR spectrophotometer and cyclic voltammetry (CV). After investigating the properties of WO₃ film, NiO film, and complementary electrochromic devices, we concluded that this device provides good reversibility, low power consumption of -2.5 V in color state, high variation of transmittance of 58.96%, changes in optical density of 0.81 and good memory effect under open-circuit conditions. In addition, electrochromic component penetration rate can be retained below 20% within 24h, showing preferred memory features; however, component coloring and bleaching response time are about 33s.

Keywords: Complementary electrochromic device, Rf-magnetron sputtered, Transmittance, Memory effect, Optical density change

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Authors: M. Hosseinnezhad, K. Gharanjig

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Natural dyes, extracted from black carrot and bramble, were utilized as photosensitizers to prepare dye-sensitized solar cells (DSSCs). Spectrophotometric studies of the natural dyes in solution and on a titanium dioxide substrate were carried out in order to assess changes in the status of the dyes. The results show that the bathochromic shift is seen on the photo-electrode substrate. The chemical binding of the natural dyes at the surface photo-electrode were increased by the chelating effect of the Ti(IV) ions. The cyclic voltammetry results showed that all extracts are suitable to be performed in DSSCs. Finally, photochemical performance and stability of DSSCs based on natural dyes were studied. The DSSCs sensitized by black carrot extract have been reported to achieve up to Jsc=1.17 mAcm^-2, Voc= 0.55 V, FF= 0.52, η=0.34%, whereas Bramble extract can obtain up to Jsc=2.24 mAcm^-2, Voc= 0.54 V, FF= 0.57, η=0.71%. The power conversion efficiency was obtained from the mixed dyes in DSSCs. The power conversion efficiency of dye-sensitized solar cells using mixed Black carrot and Bramble dye is the average of the their efficiency in single DSSCs.

Keywords: Anthocyanin, dye-sensitized solar cells, green energy, optical materials.

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Authors: N. Boshkova, K. Kamburova, N. Tabakova, N. Boshkov, Ts. Radeva

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Coatings based on polyaniline (PANI) can improve the resistance of steel against corrosion. In this work, the preparation of stable suspensions of colloidal PANI-SiO₂ particles, suitable for obtaining of composite anticorrosive coating on steel, is described. Electrokinetic data as a function of pH are presented, showing that the zeta potentials of the PANI-SiO₂ particles are governed primarily by the charged groups at the silica oxide surface. Electrosteric stabilization of the PANI-SiO₂ particles’ suspension against aggregation is realized at pH>5.5 (EB form of PANI) by adsorption of positively charged polyelectrolyte molecules onto negatively charged PANI-SiO₂ particles. The PANI-SiO₂ particles are incorporated by electrodeposition into the metal matrix of zinc in order to obtain composite (hybrid) coatings. The latter are aimed to ensure sacrificial protection of steel mainly in aggressive media leading to local corrosion damages. The surface morphology of the composite zinc coatings is investigated with SEM. The influence of PANI-SiO₂ particles on the cathodic and anodic processes occurring in the starting electrolyte for obtaining of the coatings is followed with cyclic voltammetry. The electrochemical and corrosion behavior is evaluated with potentiodynamic polarization curves and polarization resistance measurements. The beneficial effect of the stabilized PANI-SiO₂ particles for the increased protective ability of the composites is commented and discussed.

Keywords: Corrosion, polyaniline particles, zinc, protective ability.

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Authors: PoiSim Khiew, MuiYen Ho, ThianKhoonTan, WeeSiong Chiu, Roslinda Shamsudin, Muhammad Azmi Abd-Hamid, ChinHua Chia

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In the present work, we have developed a symmetric electrochemical capacitor based on the nanostructured iron oxide (Fe3O4)-activated carbon (AC) nanocomposite materials. The physical properties of the nanocomposites were characterized by Scanning Electron Microscopy (SEM) and Brunauer-Emmett-Teller (BET) analysis. The electrochemical performances of the composite electrode in 1.0 M Na2SO3 and 1.0 M Na2SO4 aqueous solutions were evaluated using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The composite electrode with 4 wt% of iron oxide nanomaterials exhibits the highest capacitance of 86 F/g. The experimental results clearly indicate that the incorporation of iron oxide nanomaterials at low concentration to the composite can improve the capacitive performance, mainly attributed to the contribution of the pseudocapacitance charge storage mechanism and the enhancement on the effective surface area of the electrode. Nevertheless, there is an optimum threshold on the amount of iron oxide that needs to be incorporated into the composite system. When this optimum threshold is exceeded, the capacitive performance of the electrode starts to deteriorate, as a result of the undesired particle aggregation, which is clearly indicated in the SEM analysis. The electrochemical performance of the composite electrode is found to be superior when Na2SO3 is used as the electrolyte, if compared to the Na2SO4 solution. It is believed that Fe3O4 nanoparticles can provide favourable surface adsorption sites for sulphite (SO3 2-) anions which act as catalysts for subsequent redox and intercalation reactions.

Keywords: Metal oxide nanomaterials, Electrochemical Capacitor, Double Layer Capacitance, Pseduocapacitance

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Authors: Nadia El Alami El Hassani, Soukaina Motia, Benachir Bouchikhi, Nezha El Bari

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Doxycycline (DXy) is a cycline antibiotic, most frequently prescribed to treat bacterial infections in veterinary medicine. However, its broad antimicrobial activity and low cost, lead to an intensive use, which can seriously affect human health. Therefore, its spread in the food products has to be monitored. The scope of this work was to synthetize a sensitive and very selective molecularly imprinted polymer (MIP) for DXy detection in honey samples. Firstly, the synthesis of this biosensor was performed by casting a layer of carboxylate polyvinyl chloride (PVC-COOH) on the working surface of a gold screen-printed electrode (Au-SPE) in order to bind covalently the analyte under mild conditions. Secondly, DXy as a template molecule was bounded to the activated carboxylic groups, and the formation of MIP was performed by a biocompatible polymer by the mean of polyacrylamide matrix. Then, DXy was detected by measurements of differential pulse voltammetry (DPV). A non-imprinted polymer (NIP) prepared in the same conditions and without the use of template molecule was also performed. We have noticed that the elaborated biosensor exhibits a high sensitivity and a linear behavior between the regenerated current and the logarithmic concentrations of DXy from 0.1 pg.mL⁻¹ to 1000 pg.mL⁻¹. This technic was successfully applied to determine DXy residues in honey samples with a limit of detection (LOD) of 0.1 pg.mL⁻¹ and an excellent selectivity when compared to the results of oxytetracycline (OXy) as analogous interfering compound. The proposed method is cheap, sensitive, selective, simple, and is applied successfully to detect DXy in honey with the recoveries of 87% and 95%. Considering these advantages, this system provides a further perspective for food quality control in industrial fields.

Keywords: Electrochemical sensor, molecular imprinted polymer, doxycycline, food control.

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Authors: B. Sadepovich Maikanov, Z. Shabanbayevich Adilbekov, R. Husainovna Mustafina, L. Tyulegenovna Auteleyeva

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This study involves detailed information about contaminants of honey in the Republic of Kazakhstan. The requirements of the technical regulation ‘Requirements to safety of honey and bee products’ and GOST 19792-2001 were taken into account in this research. Contamination of honey by antibiotics wqs determined by the IEA (immune-enzyme analysis), Ridder analyzer and Tecna produced test systems. Voltammetry (TaLab device) was used to define contamination by salts of heavy metals and gamma-beta spectrometry, ‘Progress BG’ system, with preliminary ashing of the sample of honey was used to define radioactive contamination. This article pointed out that residues of chloramphenicol were detected in 24% of investigated products, in 22% of them –streptomycin, in 7.3% - sulfanilamide, in 2.4% - tylosin, and in 12% - combined contamination was noted. Geographically, the greatest degree of contamination of honey with antibiotics occurs in the Northern Kazakhstan – 54.4%, and Southern Kazakhstan - 50%, and the lowest in Central and Eastern Kazakhstan with 30% and 25%, respectively. Generally, pollution by heavy metals is within acceptable limits, but the contamination from lead is highest in the Akmola region. The level of radioactive cesium and strontium is also within acceptable concentrations. The highest radioactivity in terms of cesium was observed in the East Kazakhstan region - 49.00±10 Bq/kg, in Akmola, North Kazakhstan and Almaty - 12.00±5, 11.05±3 and 19.0±8 Bq/kg, respectively, while the norm is 100 Bq/kg. In terms of strontium, the radioactivity in the East Kazakhstan region is 25.03±15 Bq/kg, while in Akmola, North Kazakhstan and Almaty regions it is 12.00±3, 10.2±4 and 1.0±2 Bq/kg, respectively, with the norm of 80 Bq/kg. This accumulation is mainly associated with the environmental degradation, feeding and treating of bees. Moreover, in the process of collecting nectar, external substances can penetrate honey. Overall, this research determines factors and reasons of honey contamination.

Keywords: Antibiotics, contamination of honey, honey, radionuclides.

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Authors: Maksudur Rahman Khan, Kar Min Chan, Huei Ruey Ong, Chin Kui Cheng, Wasikur Rahman

Abstract:

Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The asprepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

Keywords: Microbial fuel cell, oxygen reduction reaction, Pt/MnO2, palm oil mill effluent, polarization curve.

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