Search results for: electrochemical technique

Authors: H. Abu-Ali, A. Nabok, T. Smith

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Aptamers are single-strand of DNA or RNA nucleotides sequence which is designed in vitro using selection process known as SELEX (systematic evolution of ligands by exponential enrichment) were developed for the selective detection of many toxic materials. In this work, we have developed an electrochemical biosensor for highly selective and sensitive detection of Hg2+ and Pb2+ using a specific aptamer probe (SAP) labelled with ferrocene (or methylene blue) in (5′) end and the thiol group at its (3′) termini, respectively. The SAP has a specific coil structure that matching with G-G for Pb2+ and T-T for Hg2+ interaction binding nucleotides ions, respectively. Aptamers were immobilized onto surface of screen-printed gold electrodes via SH groups; then the cyclic voltammograms were recorded in binding buffer with the addition of the above metal salts in different concentrations. The resulted values of anode current increase upon binding heavy metal ions to aptamers and analyte due to the presence of electrochemically active probe, i.e. ferrocene or methylene blue group. The correlation between the anodic current values and the concentrations of Hg2+ and Pb2+ ions has been established in this work. To the best of our knowledge, this is the first example of using a specific DNA aptamers for electrochemical detection of heavy metals. Each increase in concentration of 0.1 μM results in an increase in the anode current value by simple DC electrochemical test i.e (Cyclic Voltammetry), thus providing an easy way of determining Hg2+ and Pb2+concentration.

Keywords: aptamer, based, biosensor, DNA, electrochemical, highly, specific

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Authors: Theo H. G. Moundzounga

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Arsenic and 2-chlorophenol are priority pollutants that pose serious health threats to humans and ecology. An electrochemical sensor, based on graphitic carbon nitride (g-C₃N₄) and carbon dots (CDs), was fabricated and used for the determination of arsenic and 2-chlorophenol. The g-C₃N₄/CDs nanocomposite was prepared via microwave irradiation heating method and was dropped-dried on the surface of the glassy carbon electrode (GCE). Transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence (PL), Fourier transform infrared spectroscopy (FTIR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) were used for the characterization of structure and morphology of the nanocomposite. Electrochemical characterization was done by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical behaviors of arsenic and 2-chlorophenol on different electrodes (GCE, CDs/GCE, and g-C₃N₄/CDs/GCE) was investigated by differential pulse voltammetry (DPV). The results demonstrated that the g-C₃N₄/CDs/GCE significantly enhanced the oxidation peak current of both analytes. The analytes detection sensitivity was greatly improved, suggesting that this new modified electrode has great potential in the determination of trace level of arsenic and 2-chlorophenol. Experimental conditions which affect the electrochemical response of arsenic and 2-chlorophenol were studied, the oxidation peak currents displayed a good linear relationship to concentration for 2-chlorophenol (R²=0.948, n=5) and arsenic (R²=0.9524, n=5), with a linear range from 0.5 to 2.5μM for 2-CP and arsenic and a detection limit of 2.15μM and 0.39μM respectively. The modified electrode was used to determine arsenic and 2-chlorophenol in spiked tap and effluent water samples by the standard addition method, and the results were satisfying. According to the measurement, the new modified electrode is a good alternative as chemical sensor for determination of other phenols.

Keywords: electrochemistry, electrode, limit of detection, sensor

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Authors: Shuo Li, Yannick Coffinier, Chann Lagadec, Fabrizio Cleri, Katsuhiko Nishiguchi, Akira Fujiwara, Soo Hyeon Kim, Nicolas Clément

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The need for single cell detection and analysis techniques has increased in the past decades because of the heterogeneity of individual living cells, which increases the complexity of the pathogenesis of malignant tumors. In the search for early cancer detection, high-precision medicine and therapy, the technologies most used today for sensitive detection of target analytes and monitoring the variation of these species are mainly including two types. One is based on the identification of molecular differences at the single-cell level, such as flow cytometry, fluorescence-activated cell sorting, next generation proteomics, lipidomic studies, another is based on capturing or detecting single tumor cells from fresh or fixed primary tumors and metastatic tissues, and rare circulating tumors cells (CTCs) from blood or bone marrow, for example, dielectrophoresis technique, microfluidic based microposts chip, electrochemical (EC) approach. Compared to other methods, EC sensors have the merits of easy operation, high sensitivity, and portability. However, despite various demonstrations of low limits of detection (LOD), including aptamer sensors, arrayed EC sensors for detecting single-cell have not been demonstrated. In this work, a new technique based on 20-nm-thick nanopillars array to support cells and keep them at ideal recognition distance for redox-labeled aptamers grafted on the surface. The key advantages of this technology are not only to suppress the false positive signal arising from the pressure exerted by all (including non-target) cells pushing on the aptamers by downward force but also to stabilize the aptamer at the ideal hairpin configuration thanks to a confinement effect. With the first implementation of this technique, a LOD of 13 cells (with5.4 μL of cell suspension) was estimated. In further, the nanosupported cell technology using redox-labeled aptasensors has been pushed forward and fully integrated into a single-cell electrochemical aptasensor array. To reach this goal, the LOD has been reduced by more than one order of magnitude by suppressing parasitic capacitive electrochemical signals by minimizing the sensor area and localizing the cells. Statistical analysis at the single-cell level is demonstrated for the recognition of cancer cells. The future of this technology is discussed, and the potential for scaling over millions of electrodes, thus pushing further integration at sub-cellular level, is highlighted. Despite several demonstrations of electrochemical devices with LOD of 1 cell/mL, the implementation of single-cell bioelectrochemical sensor arrays has remained elusive due to their challenging implementation at a large scale. Here, the introduced nanopillar array technology combined with redox-labeled aptamers targeting epithelial cell adhesion molecule (EpCAM) is perfectly suited for such implementation. Combining nanopillar arrays with microwells determined for single cell trapping directly on the sensor surface, single target cells are successfully detected and analyzed. This first implementation of a single-cell electrochemical aptasensor array based on Brownian-fluctuating redox species opens new opportunities for large-scale implementation and statistical analysis of early cancer diagnosis and cancer therapy in clinical settings.

Keywords: bioelectrochemistry, aptasensors, single-cell, nanopillars

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Authors: Tareg Omar Mansour, Khaled Omar Elhaji

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Model solutions of pentanol in the salt water of various concentrations were subjected to electrochemical oxidation using a dimensionally stable anode (DSA) and a platinised titanium cathode. The removal of pentanol was analysed over time using gas chromatography (GC) and by monitoring the total organic carbon (TOC) concentration of the reaction mixture. It was found that the removal of pentanol occurred more efficiently at higher salinities and higher applied electrical current values. When using a salt concentration of 20,000 ppm and an applied current of 100 mA there was a decrease in concentration of pentanol of 15 %. When the salt concentration and applied current were increased to 58,000 ppm and 500 mA respectively, the decrease in concentration was improved to 64 %.

Keywords: dimensionally stable anode (DSA), total organic hydrocarbon (TOC), gas chromatography mass spectrometry (GCMS), electrochemical oxidation

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Authors: Ana P. R. N. Barroso, Maurício N. Kleinberg, Frederico R. Silva, Rodrigo F. Guimarães, Marcelo M. V. Parente, Walney S. Araújo

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The fight against accelerated wear of the equipment used in the oil and gas sector is a challenge for minimizing maintenance costs. Corrosion being one of the main agents of equipment deterioration, we seek alternative materials that exhibit improved corrosion resistance at low cost of production. This study aims to evaluate the corrosion behavior of experimental alloys containing 15% and 17% of chromium (Cr) and 5% of molybdenum (Mo) in comparison with an AISI 444 commercial alloy. Microstructural analyzes were performed on samples of the alloys before and after the electrochemical tests. Two samples of each solubilized alloy were also taken for analysis of the corrosion behavior by testing potentiodynamic polarization (PP) and Electrochemical Impedance Spectroscopy (EIS) with immersion time of 24 hours in electrolytic solution with acidic character. The graphics obtained through electrochemical tests of PP and EIS indicated that among the experimental alloys, the alloy with higher chromium content (17%) had a higher corrosion resistance, confirming the beneficial effect of adding chromium. When comparing the experimental alloys with the AISI 444 commercial alloy, it is observed that the AISI 444 commercial alloy showed superior corrosion resistance to that of the experimental alloys for both assays, PP and EIS. The microstructural analyzes performed after the PP and EIS tests confirmed the results previously described. These results suggest that the addition of these levels of molybdenum did not favor the electrochemical behavior of experimental ferritic alloys for the electrolytic medium studied.

Keywords: corrosion, molybdenum, electrochemical tests, experimental alloys

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Authors: Asmae Tafraouti, Yasmina Layouni

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The fabrication of cylindrical Tungsten micro-tools with a high aspect ratio is a real challenge because of several constraints that come into during their manufacture. In this paper, we will describe the process used to fabricate these micro-tools. It consists of using electrochemical etching. We will also present the optimal protocol that makes it possible to fabricate micro-tools with a high aspect ratio in a reproducible way. Next, we will show the limit of the experimental parameters chosen to manufacture micro-tools from a wire with an initial diameter of Φ_0=250µm. The protocol used allows obtaining an average diameter of Φ=88µm ±1 µm over a length of L=3.5mm.

Keywords: drop-off effect, electrochemical etching, micro-electrical discharge machining, tungsten micro-tools

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Authors: Seval Yilmaz, Filiz Bayrakci Karel, Ali Savas Koparal

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Textile products produced by leather have been indispensable for human consumption. Various chemicals are used to enhance the durability of end-products in the processing of leather products. The wastewaters from the leather industry which contain these chemicals exhibit toxic effects on the receiving environment and threaten the natural ecosystem. In this study, leather industry wastewater (LIW), which has high loads of contaminants, was treated using advanced treatment techniques instead of conventional methods. During the experiments, the performance of electrochemical methods was investigated. During the electrochemical experiments, the performance of batch electrooxidation (EO) using boron-doped diamond (BDD) electrodes with monopolar configuration for removal of chemical oxygen demand (COD) from LIW were investigated. The influences of electrolysis time, current density (which varies as 5 mA/cm², 10 mA/cm², 20 mA/cm², 30 mA/cm², 50 mA/cm²) and initial pH (which varies as 3,80 (natural pH of LIW), 7, 9) on removal efficiency were investigated in a batch stirred cell to determine the best treatment conditions. The current density applied to the electrochemical reactors is directly proportional to the consumption of electric energy, so electrical energy consumption was monitored during the experiment. The best experimental conditions obtained in electrochemical studies were as follows: electrolysis time = 60 min, current density = 30.0 mA/cm², pH 7. Using these parameters, 53.59% COD removal rates for LIW was achieved and total energy consumption was obtained as 13.03 kWh/m³. It is concluded that electrooxidation process constitutes a plausible and developable method for the treatment of LIW.

Keywords: BDD electrodes, COD removal, electrochemical treatment, leather industry wastewater

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Authors: Fredrick O. Okumu, Mangaka C. Matoetoe

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Silver-platinum (Ag-Pt) bimetallic nanoparticles (NPs) with varying mole fractions (1:1, 1:3 and 3:1) were prepared by co-reduction of hexachloroplatinate and silver nitrate with sodium citrate. Upon successful formation of both monometallic and bimetallic (BM) core shell nanoparticles, cyclic voltammetry (CV) was used to characterize the NPs. The drop coated nanofilms on the GC substrate showed characteristic peaks of monometallic Ag NPs; Ag+/Ag0 redox couple as well as the Pt NPs; hydrogen adsorption and desorption peaks. These characteristic peaks were confirmed in the bimetallic NPs voltammograms. The following varying current trends were observed in the BM NPs ratios; GCE/Ag-Pt 1:3 > GCE/Ag-Pt 3:1 > GCE/Ag-Pt 1:1. Fundamental electrochemical properties which directly or indirectly affects the applicability of films such as; diffusion coefficient (D), electroactive surface coverage, electrochemical band gap, electron transfer coefficient (α) and charge (Q) were assessed using Randles - Sevcik plot and Laviron’s equations . High charge and surface coverage was observed in GCE/Ag-Pt 1:3 which supports its enhanced current. GCE/Ag-Pt 3:1 showed high diffusion coefficient while GCE/Ag-Pt 1:1 possessed high electron transfer coefficient that is facilitated by its high apparent heterogeneous rate constant relative to other BM NPs ratios. Surface redox reaction was determined as adsorption controlled in all modified GCEs. Surface coverage is inversely proportional to size; therefore the surface coverage data suggests that Ag-Pt 1:1 NPs have a small particle size. Generally, GCE/Ag-Pt 1:3 depicts the best electrochemical properties.

Keywords: characterization, core-shell, electrochemical, nanoparticles

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Authors: Megha, Diksha, Seema Rani, Balwinder Kaur, Harminder Kaur

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Fe₃O₄@SiO₂@SB functionalized magnetic nanoparticles were synthesized and used to detect heavy metal ions such as Pb²⁺, Hg²⁺, and Cd²⁺ in water. The formation of Fe₃O₄@SiO₂@SB nanocatalyst was confirmed by XRD, SEM, TEM, and IR. The simultaneous determination of analyte cations was carried out using square wave anodic stripping voltammetry (SWASV). Investigation and optimisation were done to study how experimental variables affected the performance of the modified magnetic electrode. Pb²⁺, Hg²⁺, and Cd²⁺ were successfully detected using the designed sensor in the presence of various possibly interfering ions. The recovery rate was found to be 97.5% for Pb²⁺, 96.2% for Hg²⁺, 103.5% for Cd²⁺. The electrochemical sensor was also employed to determine the presence of heavy metal ions in drinking water samples, which are well below the World Health Organization (WHO) guidelines.

Keywords: magnetic nanoparticles, heavy metal ions, electrochemical sensor, environmental water samples

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Authors: Abdur Rahim, Lauro Tatsuo Kubota, Yoshitaka Gushikem

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Carbon ceramic mesoporous SiO2/50wt%C (SBET= 170 m2g-1), where C is graphite, was prepared by the sol gel method. Scanning electron microscopy images and the respective element mapping showed that, within the magnification used, no phase segregation was detectable. It presented the electric conductivities of 0.49 S cm-1. This material was used to support cobalt phthalocyanine, prepared in situ, to assure a homogeneous dispersion of the electro active complex in the pores of the matrix. The surface density of cobalt phthalocyanine, on the matrix surfaces was 0.015 mol cm-2. Pressed disk, made with SiO2/50wt%C/CoPc, was used to fabricate an electrode and tested as sensors for nitrite determination by electro chemical technique. A linear response range between 0.039 and 0.42 mmol l−1,and correlation coefficient r=0.9996 was obtained. The electrode was chemically very stable and presented very high sensitivity for this analyte, with a limit of detection, LOD = 1.087 x 10-6 mol L-1.

Keywords: SiO2/C/CoPc, sol-gel method, electrochemical sensor, nitrite oxidation, carbon ceramic material, cobalt phthalocyanine

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Authors: A. Hamam, D. Oukil, A. Dib, L. Makhloufi

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The aim of this work is to synthesize modified Polypyrrole films (PPy) containing nanoparticles of copper oxides onto a non conducting cellulosic substrate. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is carried out using FeCl3 as an oxidant and Pyrrole as monomer. Different parameters were optimized (monomer concentration, duration of the experiment, nature of supporting electrolyte, temperature, etc.) in order to obtain films with different thickness and different morphologies. Thickness and topography of different PPy deposits were estimated by a profilometer apparatus. The electrochemical reactivity of the obtained electrodes were tested by cyclic voltammetry technique (CV) and electrochemical impedance spectroscopy (EIS). Secondly, the modification of the PPy film surface by incorporation of copper oxide nanonoparticles is conducted by applying a galvanostatic procedure from CuCl2 solution. Surface characterization has been carried out using scanning microscope (SEM) coupled with energy dispersive X-ray analysis (EDX), Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis showed the presence of the copper oxide nanoparticles (CuO) in the polymer films with dimensions less than 50 nm.

Keywords: polypyrrole, modified electrode, cellulosic substrate, copper oxide

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Authors: B. D. Polat, Ö. Keleş

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Physical vapor deposition under conditions of an obliquely incident flux results in a film formation with an inclined columnar structure. These columns will be oriented toward the vapor source because of the self-shadowing effect, and they are homogenously distributed on the substrate surface because of the limited surface diffusion ability of ad-atoms when there is no additional substrate heating. In this work, the oblique angle electron beam evaporation technique is used to fabricate thin films containing inclined nanorods. The results demonstrate that depending on the thin film composition, the morphology of the nanorods changed as well. The galvanostatic analysis of these thin film anodes reveals that a composite CuSn nanorods having approximately 900mAhg-1 of initial discharge capacity, performs higher electrochemical performance compared to pure Sn nanorods containing anode material. The long cycle life and the advanced electrochemical properties of the nano-structured composite electrode might be attributed to its improved mechanical tolerance and enhanced electrical conductivity depending on the Cu presence in the nanorods.

Keywords: Cu-Sn thin film, oblique angle deposition, lithium ion batteries, anode

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Authors: Basanti Ekka, Talis Juhna

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Dairy industrial effluents originated by the typical processing activities are composed of various organic and inorganic constituents, and these include proteins, fats, inorganic salts, antibiotics, detergents, sanitizers, pathogenic viruses, bacteria, etc. These contaminants are harmful to not only human beings but also aquatic flora and fauna. Because consisting of large classes of contaminants, the specific targeted removal methods available in the literature are not viable solutions on the industrial scale. Therefore, in this on-going research, a series of coagulation, electrochemical, and catalytic methods will be employed. The bulk coagulation and electrochemical methods can wash off most of the contaminants, but some of the harmful chemicals may slip in; therefore, specific catalysts designed and synthesized will be employed for the removal of targeted chemicals. In the context of Latvian dairy industries, presently, work is under progress on the characterization of dairy effluents by total organic carbon (TOC), Inductively Coupled Plasma Mass Spectrometry (ICP-MS)/ Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), High-Performance Liquid Chromatography (HPLC), Gas Chromatography-Mass Spectrometry (GC-MS), and Mass Spectrometry. After careful evaluation of the dairy effluents, a cost-effective natural coagulant will be employed prior to advanced electrochemical technology such as electrocoagulation and electro-oxidation as a secondary treatment process. Finally, graphene oxide (GO) based hybrid materials will be used for post-treatment of dairy wastewater as graphene oxide has been widely applied in various fields such as environmental remediation and energy production due to the presence of various oxygen-containing groups. Modified GO will be used as a catalyst for the removal of remaining contaminants after the electrochemical process.

Keywords: catalysis, dairy wastewater, electrochemical method, graphene oxide

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Authors: Dahmane Mohamed, Tab Asma, Trari Mohamed

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BaMnO₃ nanoparticles were synthesized by a nitrate route. Its structure and physical properties were characterized by means of X-ray powder diffraction, radio crystallographic analysis, ultraviolet-visible absorption spectroscopy in diffuse reflectance mode, infrared spectroscopy, and electrochemical measurements. The optical study showed that barium manganese oxide presents a direct transition with band energy 2.13 eV. The electrochemical study allowed us to identify the redox peaks and the corrosion parameters. Capacitance measurement clearly showed n-type conductivity. The photodegradation of paracetamol by BaMnO₃ was followed by UV-visible spectrophotometry; the results were then confirmed by HPLC. BaMnO₃ has shown its photocatalytic efficiency in the photodegradation of 10 mg/L paracetamol under solar irradiation, with a yield of ≈ 88%. The kinetic study has shown that paracetamol degrades with first-order kinetics.

Keywords: BaMnO₃, photodegradation, paracetamol, electrochemical measurements, solar light

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Authors: Usha N. Murthy, H. B. Rekha, Mahaveer Devoor

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The introduction of more stringent pollution regulations, in relation to financial and social pressures for sustainable development, has pressed toward limiting the volumes of industrial and domestic effluents discharged into the environment-as well as to increase the efforts within research and development of new or more efficient wastewater treatment technologies. Considering both discharge volume and effluent composition, wastewater generated by the textile industry is rated as the most polluting among all industrial sectors. The pollution load is mainly due to spent dye baths, which are composed of unreacted dyes, dispersing agents, surfactants, salts and organics. In the present investigation, the textile dye wastewater was characterized by high colour, chemical oxygen demand (COD), total dissolved solids (TDS) and pH. Electrochemical oxidation process for four plate electrodes was carried out at five different current intensities, out of which 0.14A has achieved maximum percentage removal of COD with 75% and 83% of colour. The COD removal rate in kg COD/h/m2 decreases with increase in the current intensity. The energy consumption increases with increase in the current intensity. Hence, textile dye wastewater can be effectively pre-treated by electrochemical oxidation method where the process limits objectionable colour while leaving the COD associated with organics left for natural degradation thus causing a sustainable reduction in pollution load.

Keywords: electrochemical treatment, COD, colour, environmental engineering

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Authors: Angelo Gabriel Buenaventura, Allan Christopher Yago

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A carbon paste electrode (CPE) composed of Multiwalled Carbon Nanotube (MWCNT) conducting particle and Polydimethylsiloxane (PDMS) binder was used for simultaneous detection of Dopamine (DA) and Uric Acid (UA) in the presence of Ascorbic Acid (AA) at physiological level. The MWCNT-PDMS CPE was initially activated via potentiodynamic cycling in a basic (NaOH) solution, which resulted in enhanced electrochemical properties. Electrochemical Impedance Spectroscopy measurements revealed a significantly lower charge transfer resistance (Rct) for the OH--activated MWCNT-PDMS CPE (Rct = 5.08kΩ) as compared to buffer (pH 7)-activated MWCNT-PDMS CPE (Rct = 25.9kΩ). Reversibility analysis of Fe(CN)63-/4- redox couple of both Buffer-Activated CPE and OH--Activated CPE showed that the OH—Activated CPE have peak current ratio (Ia/Ic) of 1.11 at 100mV/s while 2.12 for the Buffer-Activated CPE; this showed an electrochemically reversible behavior for Fe(CN)63-/4- redox couple even at relatively fast scan rate using the OH--activated CPE. Enhanced voltammetric signal for DA and significant peak separation between DA and UA was obtained using the OH--activated MWCNT-PDMS CPE in the presence of 50 μM AA via Differential Pulse Voltammetry technique. The anodic peak currents which appeared at 0.263V and 0.414 V were linearly increasing with increasing concentrations of DA and UA, respectively. The linear ranges were obtained at 25 μM – 100 μM for both DA and UA. The detection limit was determined to be 3.86 μM for DA and 5.61 μM for UA. These results indicate a practical approach in the simultaneous detection of important bio-organic molecules using a simple CPE composed of MWCNT and PDMS with base anodization as activation technique.

Keywords: anodization, ascorbic acid, carbon paste electrodes, dopamine, uric acid

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Authors: Alex Soares Castro, Matheus Manoel Teles de Menezes, Larissa Silva de Azevedo, Ana Carolina Caleffi Patelli, Osmair Vital de Oliveira, Aline Thais Bruni, Marcelo Firmino de Oliveira

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Considering the problem of the seizure of illicit drugs, as well as the development of electrochemical sensors using chemically modified electrodes, this work shows the study of the electrochemical activity of cocaine in carbon paste electrode chemically modified with Cu (II) trans 3-MeO salcn complex. In this context, cyclic voltammetry was performed on 0.1 mol.L⁻¹ KCl supporting electrolyte at a scan speed of 100 mV s⁻¹, using an electrochemical cell composed of three electrodes: Ag /AgCl electrode (filled KCl 3 mol.L⁻¹) from Metrohm® (reference electrode); a platinum spiral electrode, as an auxiliary electrode, and a carbon paste electrode chemically modified with Cu (II) trans 3-MeO complex (as working electrode). Two forms of cocaine were analyzed: cocaine hydrochloride (pH 3) and cocaine free base form (pH 8). The PM7 computational method predicted that the hydrochloride form is more stable than the free base form of cocaine, so with cyclic voltammetry, we found electrochemical signal only for cocaine in the form of hydrochloride, with an anodic peak at 1.10 V, with a linearity range between 2 and 20 μmol L⁻¹ had LD and LQ of 2.39 and 7.26x10-5 mol L⁻¹, respectively. The study also proved that cocaine is adsorbed on the surface of the working electrode, where through an irreversible process, where only anode peaks are observed, we have the oxidation of cocaine, which occurs in the hydrophilic region due to the loss of two electrons. The mechanism of this reaction was confirmed by the ab-inito quantum method.

Keywords: ab-initio computational method, analytical method, cocaine, Schiff base complex, voltammetry

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Authors: Md. Abdul Aziz

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Sulfide ion is water soluble, highly corrosive, toxic and harmful to the human beings. As a result, knowing the exact concentration of sulfide in water is very important. However, the existing detection and quantification methods have several shortcomings, such as high cost, low sensitivity, and massive instrumentation. Consequently, the development of novel sulfide sensor is relevant. Nevertheless, electrochemical methods gained enormous popularity due to a vast improvement in the technique and instrumentation, portability, low cost, rapid analysis and simplicity of design. Successful field application of electrochemical devices still requires vast improvement, which depends on the physical, chemical and electrochemical aspects of the working electrode. The working electrode made of bulk gold (Au) and platinum (Pt) are quite common, being very robust and endowed with good electrocatalytic properties. High cost, and electrode poisoning, however, have so far hindered their practical application in many industries. To overcome these obstacles, we developed a sulfide sensor based on an indium tin oxide nanoparticle (ITONP)-modified ITO electrode. To prepare ITONP-modified ITO, various methods were tested. Drop-drying of ITONPs (aq.) on aminopropyltrimethoxysilane-functionalized ITO (APTMS/ITO) was found to be the best method on the basis of voltammetric analysis of the sulfide ion. ITONP-modified APTMS/ITO (ITONP/APTMS/ITO) yielded much better electrocatalytic properties toward sulfide electro-οxidation than did bare or APTMS/ITO electrodes. The ITONPs and ITONP-modified ITO were also characterized using transmission electron microscopy and field emission scanning electron microscopy, respectively. Optimization of the type of inert electrolyte and pH yielded an ITONP/APTMS/ITO detector whose amperometrically and chronocoulοmetrically determined limits of detection for sulfide in aqueous solution were 3.0 µM and 0.90 µM, respectively. ITONP/APTMS/ITO electrodes which displayed reproducible performances were highly stable and were not susceptible to interference by common contaminants. Thus, the developed electrode can be considered as a promising tool for sensing sulfide.

Keywords: amperometry, chronocoulometry, electrocatalytic properties, ITO-nanoparticle-modified ITO, sulfide sensor

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Authors: Aliya Kurbanova, Nurlan Akhmetov, Abilmansur Yeshmuratov, Yerzhigit Sugurbekov, Ramiz Zulkharnay, Gulzat Demeuova, Murat Baisariyev, Gulnar Sugurbekova

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Last decades crude oils have tended to become more challenge to process due to increasing amounts of sour and heavy crude oils. Some crude oils contain high vanadium and nickel content, for example Pavlodar LLP crude oil, which contains more than 23.09 g/t nickel and 58.59 g/t vanadium. In this study, we used two types of metal removing methods such as solvent extraction and electrochemical. The present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Applying the cyclic voltametric analysis (CVA) and Inductively coupled plasma mass spectrometry (ICP MS), these mentioned types of metal extraction methods were compared in this paper. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for nickel and 51.2% for vanadium content from crude oil. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits into the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V.

Keywords: demetallization, deasphalting, electrochemical removal, heavy metals, petroleum engineering, solvent extraction

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Authors: Wei-Bo Hua, Zhuo Zheng, Xiao-Dong Guo, Ben-He Zhong

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The layered structure LiNi1/3Co1/3Mn1/3-xAlxO2 (x = 0 ~ 0.04) series cathode materials were synthesized by a carbonate co-precipitation method, followed by a high temperature calcination process. The influence of Al substitution on the microstructure and electrochemical performances of the prepared materials was investigated by X-Ray diffraction (XRD), scanning electron microscopy (SEM), and galvanostatic charge/discharge test. The results show that the LiNi1/3Co1/3Mn1/3-xAlxO2 has a well-ordered hexagonal "α" -NaFeO2 structure. Although the discharge capacity of Al-doped samples decreases as x increases, LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 exhibits superior capacity retention at high voltage (4.6 V). Therefore, LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 is a promising material for “green” vehicles.

Keywords: lithium ion battery, carbonate co-precipitation, doping, microstructure, electrochemical properties

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Authors: Zahrasadat Hosseini, Jie Yuan

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Point-of-care (POC) diagnostic devices based on lab-on-a-chip (LOC) technology have the potential to revolutionize medical diagnostics. However, the development of an ideal microfluidic system based on LOC technology for diagnostics purposes requires overcoming several obstacles, such as improving sensitivity, selectivity, portability, cost-effectiveness, and prototyping methods. While numerous studies have introduced technologies and systems that advance these criteria, existing systems still have limitations. Electrochemical enzyme-linked immunosorbent assay (e-ELISA) in a LOC device offers numerous advantages, including enhanced sensitivity, decreased turnaround time, minimized sample and analyte consumption, reduced cost, disposability, and suitability for miniaturization, integration, and multiplexing. In this study, we present a novel design and fabrication method for a microfluidic diagnostic platform that integrates screen-printed electrochemical carbon/silver chloride electrodes on flexible printed circuit boards with flexible, multilayer, polydimethylsiloxane (PDMS) microfluidic networks to accurately manipulate and pre-immobilize analytes for performing electrochemical enzyme-linked immunosorbent assay (e-ELISA) for multiplexed quantification of blood serum biomarkers. We further demonstrate fast, cost-effective prototyping, as well as accurate and reliable detection performance of this device for quantification of interleukin-6-spiked samples through electrochemical analytics methods. We anticipate that our invention represents a significant step towards the development of user-friendly, portable, medical-grade, POC diagnostic devices.

Keywords: lab-on-a-chip, point-of-care diagnostics, electrochemical ELISA, biomarker quantification, fast prototyping

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Authors: Zahrasadat Hosseini, Jie Yuan

Abstract:

Point-of-care (POC) diagnostic devices based on lab-on-a-chip (LOC) technology have the potential to revolutionize medical diagnostics. However, the development of an ideal microfluidic system based on LOC technology for diagnostics purposes requires overcoming several obstacles, such as improving sensitivity, selectivity, portability, cost-effectiveness, and prototyping methods. While numerous studies have introduced technologies and systems that advance these criteria, existing systems still have limitations. Electrochemical enzyme-linked immunosorbent assay (e-ELISA) in a LOC device offers numerous advantages, including enhanced sensitivity, decreased turnaround time, minimized sample and analyte consumption, reduced cost, disposability, and suitability for miniaturization, integration, and multiplexing. In this study, we present a novel design and fabrication method for a microfluidic diagnostic platform that integrates screen-printed electrochemical carbon/silver chloride electrodes on flexible printed circuit boards with flexible, multilayer, polydimethylsiloxane (PDMS) microfluidic networks to accurately manipulate and pre-immobilize analytes for performing electrochemical enzyme-linked immunosorbent assay (e-ELISA) for multiplexed quantification of blood serum biomarkers. We further demonstrate fast, cost-effective prototyping, as well as accurate and reliable detection performance of this device for quantification of interleukin-6-spiked samples through electrochemical analytics methods. We anticipate that our invention represents a significant step towards the development of user-friendly, portable, medical-grade POC diagnostic devices.

Keywords: lab-on-a-chip, point-of-care diagnostics, electrochemical ELISA, biomarker quantification, fast prototyping

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Authors: Shekher Kummari, V. Sunil Kumar, K. Vengatajalabathy Gobi

Abstract:

A simple, cost-effective, reusable and reagent-free electrochemical biosensor is developed with functionalized multiwall carbon nanotube paste electrode (f-CNTPE) for the sensitive and selective determination of the important chemotherapeutic drug methotrexate (MTX), which is widely used for the treatment of various cancer and autoimmune diseases. The electrochemical response of the fabricated electrode towards the detection of MTX is examined by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV). CV studies have shown that f-CNTPE electrode system exhibited an excellent electrocatalytic activity towards the oxidation of MTX in phosphate buffer (0.2 M) compared with a conventional carbon paste electrode (CPE). The oxidation peak current is enhanced by nearly two times in magnitude. Applying the DPV method under optimized conditions, a linear calibration plot is achieved over a wide range of concentration from 4.0×10⁻⁷ M to 5.5×10⁻⁶ M with the detection limit 1.6×10⁻⁷ M. further, by applying the SWV method a parabolic calibration plot was achieved starting from a very low concentration of 1.0×10⁻⁸ M, and the sensor could detect as low as 2.9×10⁻⁹ M MTX in 10 s and 10 nM were detected in steady state current-time analysis. The f-CNTPE shows very good selectivity towards the specific recognition of MTX in the presence of important biological interference. The electrochemical biosensor detects MTX in-vitro directly from pharmaceutical sample, undiluted urine and human blood serum samples at a concentration range 5.0×10⁻⁷ M with good recovery limits.

Keywords: amperometry, electrochemical detection, human blood serum, methotrexate, MWCNT, SWV

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Authors: Nadia Hammouda, Kamel Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, seawater

Procedia PDF Downloads 386

Authors: Nadia Hammouda, K. Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, sea water

Procedia PDF Downloads 445

Authors: Abdullah Faqihi, John Hedley

Abstract:

Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: laser scribing, lightscribe DVD, graphene oxide, scanning electron microscopy

Procedia PDF Downloads 91

Authors: R. Khrifou, M. Galai, R. Touir, M. Ebn Touhami, Y. Ramli

Abstract:

A 2-(5-methyl-2-Nitro-1H-imidazol-1-yl)ethyl benzoate (IMDZ-B) was synthesized and characterized using elemental analyses, NMR, and Fourier transform infrared (FTIR) techniques. Its effect on brass corrosion in 1.0 M H₃PO₄ solution was investigated by using electrochemical measurements coupled with X-ray diffraction analysis (XRD), Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX). The polarization measurements showed that the IMDZ-B acts as a mixed-type inhibitor. Indeed, it is found that the IMDZ-B compound is a very good inhibitor, and its inhibition efficiency increases with concentration to reach a maximum of 99.5 % at 10-³ M. In addition, the obtained electrochemical parameters from impedance indicated that the IMDZ-B molecules act by adsorption on metallic surfaces. This adsorption was found to obey Langmuir’s adsorption isotherm. However, the temperature effect on the performance of IMDZ-B was also studied. It is found that the IMDZ-B takes its performance at high temperatures. In addition, the obtained kinetic and thermodynamic parameters showed that the IMDZ-B molecules act via two adsorption modes, physisorption and chemisorptions, and its process is endothermic and spontaneous. Finally, the XRD and SEM/EDX analyses confirmed the electrochemical obtained results.

Keywords: low concentration, anti-corrosion brass, IMDZ-B product, phosphoric acid solution, electrochemical, SEM\EDAX analysis

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Authors: Girish Sambhaji Gund

Abstract:

The controlled nanostructure growth and its strong coupling with the current collector are key factors to achieve good electrochemical performance of faradaic-dominant electroactive materials. We employed binder-less and additive-free hydrothermal and physical vapor doping methods for the synthesis of nickel (Ni) and cobalt (Co) based compounds nanostructures (NiO, NiCo2O4, NiCo2S4) deposited on different conductive substrates such as carbon nanotube (CNT) on stainless steel, and reduced graphene oxide (rGO) and N-doped rGO on nickel foam (NF). The size and density of Ni- and Co-based compound nanostructures are controlled through the strong coupling with carbon allotropes on stainless steel and NF substrates. This controlled nanostructure of Ni- and Co-based compounds with carbon allotropes leads to stable faradaic electrochemical reactions at the material/current collector interface and within the electrode, which is consequence of strong coupling of nanostructure with functionalized carbon surface as a buffer layer. Thus, it is believed that the results provide the synergistic approaches to stabilize electrode materials physically and chemically, and hence overall electrochemical activity of faradaic dominating battery-type electrode materials through buffer layer engineering.

Keywords: metal compounds, carbon allotropes, doping, electrochemicstry, hybrid supercapacitor

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Authors: M. El Hajji, A. Hallaoui, L. Bazzi, A. Benlhachemi, O. Jbara, A. Tara, B. Bakiz, L. Bazzi, M. Hilali

Abstract:

The objective of this study was the development of zinc-copper binary oxide "Cu2O-ZnO" thin films by the electrochemical method "cathodic electrodeposition" and their uses for the degradation of a basic dye "Congo Red" by direct anodic oxidation. The anode materials synthesized were characterized by X-ray diffraction "XRD" and by scanning electron microscopy "SEM" coupled to EDS.

Keywords: Cu2O-ZnO thin films, cathodic electrodeposition, electrodegradation, Congo Red, BDD

Procedia PDF Downloads 323

Authors: Sharan K. Indrakar, Aakash B. Prasad, Arash Takshi, Sesha Srinivasan, Elias K. Stefanakos

Abstract:

In this work, we present an exclusive study on the effect of the feeding ratio of polyaniline-based redox-active gel layer on electrical and optical properties of innovative electrochromic devices (ECs). An electrochromic device consisting of polyaniline (PANI) has a redox-active gel electrolyte placed between two conducting transparent fluorine-doped tin oxide glass substrates. The redox-active composite gel is a mixture of different concentrations of aniline (monomer), a water-soluble polymer poly (vinyl alcohol), hydrochloric acid, and an oxidant. The EC device shows the color change from dark green to transparent for the applied potential between -0.5 V to +2.0 V. The coloration and decoloration of the ECs were tested for electrochemical behavior using techniques such as cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS). The optical transparency of the EC devices was examined at two different biasing voltage conditions under UV-visible spectroscopic technique; the result showed 65% transmittance at 564 nm and zero transmittance when the cell was biased at 0.0 V and 2.0 V, the synthesized mol fraction gel was analyzed for surface morphology and structural properties by scanning electron microscopy and Fourier transformer spectroscopy.

Keywords: electrochromic, gel electrolyte, polyaniline, conducting polymer

Procedia PDF Downloads 105