Search results for: electrochemical impedence spectroscopy

Authors: Mandlenkosi George Robert Mahlobo, Tumelo Seadira, Major Melusi Mabuza, Peter Apata Olubambi

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Cathodic protection (CP) has been widely considered a suitable technique for mitigating corrosion of buried metal structures. Plenty of efforts have been made in developing techniques, in particular non-destructive techniques, for monitoring and quantifying the effectiveness of CP to ensure the sustainability and performance of buried steel structures. The aim of this study was to investigate the evolution of the electrochemical processes at the steel/soil interface during the application of CP on steel in simulated soil. Carbon steel was subjected to electrochemical tests with NS4 solution used as simulated soil conditions for 4 days before applying CP for a further 11 days. A previously modified non-destructive voltammetry technique was applied before and after the application of CP to measure the corrosion rate. Electrochemical impedance spectroscopy (EIS), in combination with mathematical modeling through equivalent electric circuits, was applied to determine the electrochemical behavior at the steel/soil interface. The measured corrosion rate was found to have decreased from 410 µm/yr to 8 µm/yr between days 5 and 14 because of the applied CP. Equivalent electrical circuits were successfully constructed and used to adequately model the EIS results. The modeling of the obtained EIS results revealed the formation of corrosion products via a mixed activation-diffusion mechanism during the first 4 days, while the activation mechanism prevailed in the presence of CP, resulting in a protective film. The x-ray diffraction analysis confirmed the presence of corrosion products and the predominant protective film corresponding to the calcareous deposit.

Keywords: carbon steel, cathodic protection, NS4 solution, voltammetry, EIS

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Authors: S. N. Hussain, H. M. A. Asghar, H. Sattar, E. P. L. Roberts

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Arvia™ introduced a novel technology consisting of adsorption followed by electrochemical regeneration with a graphite intercalation compound adsorbent that takes place in a single unit. The adsorbed species may lead to the formation of intermediate by-products products due to incomplete mineralization during electrochemical regeneration. Therefore, the investigation of breakdown products due to incomplete oxidation is of great concern regarding the commercial applications of this process. In the present paper, the formation of the chlorinated breakdown products during continuous process of adsorption and electrochemical regeneration based on a graphite intercalation compound adsorbent has been investigated.

Keywords: GIC, adsorption, electrochemical regeneration, chlorphenols

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Authors: Zohreh Derikvand

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One new 2D metal-organic coordination polymer of Ni(II) namely [Ni2(ndc)2(DMSO)4(H2O)]n, where ndc = naphthalene-1,4-dicarboxylic acid and DMSO= dimethyl sulfoxide has been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. Compound 1 possesses a 2D layer structure constructed from dinuclear nickel(II) building blocks in which two crystallographically independent Ni2+ ions are bridged by ndc2– ligands and water molecule. The ndc2– ligands adopt μ3 bridging modes, linking the metal centers into a two-dimensional coordination framework. The two independent NiII cations are surrounded by dimethyl sulfoxide and naphthalene-1,4-dicarboxylate molecules in distorted octahedron geometry. In the crystal structures of 1 there are non-classical hydrogen bonding arrangements and C-H–π stacking interactions. Electrochemical behavior of [Ni2(ndc)2(DMSO)4(H2O)]n, (Ni-NDA) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) was described. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). Oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) and the results showed that the Ni-NDA/CNTs film displays excellent electrochemical catalytic activities towards fructose oxidation.

Keywords: naphthalene-1, 4-dicarboxylic acid, crystal structure, coordination polymer, electrocatalysis, impedance spectroscopy

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Authors: Tian-Fang Kang, Chao-Nan Ge, Rui Li

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An electrochemical biosensor for the determination of organophosphorus pesticides was developed based on electrochemical co-deposition of Au and Pd nanoparticles on glassy carbon electrode (GCE). Energy disperse spectroscopy (EDS) analysis was used for characterization of the surface structure. Scanning electron micrograph (SEM) demonstrates that the films are uniform and the nanoclusters are homogeneously distributed on the GCE surface. Acetylcholinesterase (AChE) was immobilized on the Au and Pd nanoparticle modified electrode (Au-Pd/GCE) by cross-linking with glutaraldehyde. The electrochemical behavior of thiocholine at the biosensor (AChE/Au-Pd/GCE) was studied. The biosensors exhibited substantial electrocatalytic effect on the oxidation of thiocholine. The peak current of linear scan voltammetry (LSV) of thiocholine at the biosensor is proportional to the concentration of acetylthiocholine chloride (ATCl) over the range of 2.5 × 10-6 to 2.5 × 10-4 M in 0.1 M phosphate buffer solution (pH 7.0). The percent inhibition of acetylcholinesterase was proportional to the logarithm of parathion concentration in the range of 4.0 × 10-9 to 1.0 × 10-6 M. The detection limit of parathion was 2.6 × 10-9 M. The proposed method exhibited high sensitivity and good reproducibility.

Keywords: acetylcholinesterase, Au-Pd nanoparticles, electrochemical biosensors, parathion

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Authors: Meltem Agar, Maisem Laabei, Hannah Leese, Pedro Estrela

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Pathogenic bacteria and the diseases they cause have become a global problem. Their early detection is vital and can only be possible by detecting the bacteria causing the disease accurately and rapidly. Great progress has been made in this field with the use of biosensors. Molecularly imprinted polymers have gain broad interest because of their excellent properties over natural receptors, such as being stable in a variety of conditions, inexpensive, biocompatible and having long shelf life. These properties make molecularly imprinted polymers an attractive candidate to be used in biosensors. In this study it is aimed to produce an aptamer-molecularly imprinted polymer based electrochemical sensor by utilizing the properties of molecularly imprinted polymers coupled with the enhanced specificity offered by DNA aptamers. These ‘apta-MIP’ sensors were used for the detection of Staphylococcus aureus and Escherichia coli. The experimental parameters for the fabrication of sensor were optimized, and detection of the bacteria was evaluated via Electrochemical Impedance Spectroscopy. Sensitivity and selectivity experiments were conducted. Furthermore, molecularly imprinted polymer only and aptamer only electrochemical sensors were produced separately, and their performance were compared with the electrochemical sensor produced in this study. Aptamer-molecularly imprinted polymer based electrochemical sensor showed good sensitivity and selectivity in terms of detection of Staphylococcus aureus and Escherichia coli. The performance of the sensor was assessed in buffer solution and tap water.

Keywords: aptamer, electrochemical sensor, staphylococcus aureus, molecularly imprinted polymer

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Authors: Rafiuddin

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Composite solid electrolyte of the salt and oxide type is an effective approach to improve the ionic conductivity in low and intermediate temperature regions. The conductivity enhancement in the composites occurs via interfaces. Because of their high ionic conduction, composite electrolytes have wide applications in different electrochemical devices such as solid-state batteries, solid oxide fuel cells, and electrochemical cells. In this work, a series of novel (1‒x) (CdI2‒Ag2CrO4)‒xAl2O3 composite solid electrolytes has been synthesized. The prepared materials were characterized by X‒ray diffraction, differential thermal analysis, and AC impedance spectroscopy. The impedance spectra show single semicircle representing the simultaneous contribution of grain and grain boundary. The conductivity increased with the increase of Al2O3 content and shows the maximum conductivity (σ= 0.0012 S cm‒1) for 30% of Al2O3 content at 30 ℃.

Keywords: composite solid electrolyte, X-ray diffraction, Impedance spectroscopy, ionic conductivity

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Authors: Yongkui Cui, Fengping Wang, Hailei Zhao, Muhammad Zubair Iqbal, Ziya Wang, Yan Li, Pengpeng LV

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The novel 3D SnO cabbages self-assembled by nanosheets were successfully synthesized via template-free hydrothermal growth method under facile conditions.The XRD results manifest that the as-prepared SnO is tetragonal phase. The TEM and HRTEM results show that the cabbage nanosheets are polycrystalline structure consisted of considerable single-crystalline nanoparticles. Two typical Raman modes A1g=210 and Eg=112 cm-1 of SnO are observed by Raman spectroscopy. Moreover, galvanostatic cycling tests has been performed using the SnO cabbages as anode material of lithium ion battery and the electrochemical results suggest that the synthesized SnO cabbage structures are a promising anode material for lithium ion batteries.

Keywords: electrochemical property, hydrothermal synthesis, lithium ion battery, stannous oxide

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Authors: S. B. Mayil Vealan, C. Sekar

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Bisphenol A (BIS A) and 4 Nitrophenol (4N) are the most prevalent environmental endocrine-disrupting chemicals which mimic hormones and have a direct relationship to the development and growth of animal and human reproductive systems. Moreover, intensive exposure to the compound is related to prostate and breast cancer, infertility, obesity, and diabetes. Hence, accurate and reliable determination techniques are crucial for preventing human exposure to these harmful chemicals. Lanthanum Copper Oxide (La₂Cu₂O₅) nanoparticles were synthesized and investigated through various techniques such as scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. Cyclic voltammetry and square wave voltammetry techniques are employed to evaluate the electrochemical behavior of as-synthesized samples toward the electrochemical detection of Bisphenol A and 4-Nitrophenol. Under the optimal conditions, the oxidation current increased linearly with increasing the concentration of BIS A and 4-N in the range of 0.01 to 600 μM with a detection limit of 2.44 nM and 3.8 nM. These are the lowest limits of detection and the widest linear ranges in the literature for this determination. The method was applied to the simultaneous determination of BIS A and 4-N in real samples (food packing materials and river water) with excellent recovery values ranging from 95% to 99%. Better stability, sensitivity, selectivity and reproducibility, fast response, and ease of preparation made the sensor well-suitable for the simultaneous determination of bisphenol and 4 Nitrophenol. To the best of our knowledge, this is the first report in which La₂Cu₂O₅ nano particles were used as efficient electron mediators for the fabrication of endocrine disruptor (BIS A and 4N) chemical sensors.

Keywords: endocrine disruptors, electrochemical sensor, Food contacting materials, lanthanum cuprates, nanomaterials

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Authors: Abebe Taye

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The interest in enhancing the performance of all-solid-state batteries featuring lithium metal anodes as a potential alternative to traditional lithium-ion batteries has prompted exploration into new avenues. A promising strategy involves transforming lithium-ion batteries into hybrid configurations by integrating lithium-ion and lithium-metal solid-state components. This study is focused on achieving stable lithium deposition and advancing the electrochemical capabilities of solid-state lithium hybrid batteries with anodes by incorporating mesocarbon microbeads (MCMBs) blended with silver nanoparticles. To achieve this, mesocarbon microbeads (MCMBs) blended with silver nanoparticles are coated on stainless-steel current collectors. These samples undergo a battery of analyses employing diverse techniques. Surface morphology is studied through scanning electron microscopy (SEM). The electrochemical behavior of the coated samples is evaluated in both half-cell and full-cell setups utilizing an argyrodite-type sulfide electrolyte. The stability of MCMBs in the electrolyte is assessed using electrochemical impedance spectroscopy (EIS). Additional insights into the composition are gleaned through X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). At an ultra-low N/P ratio of 0.26, stability is upheld for over 100 charge/discharge cycles in half-cells. When applied in a full-cell configuration, the hybrid anode preserves 60.1% of its capacity after 80 cycles at 0.3 C under a low N/P ratio of 0.45. In sharp contrast, the capacity retention of the cell using untreated MCMBs declines to 20.2% after a mere 60 cycles. The introduction of mesocarbon microbeads (MCMBs) combined with silver nanoparticles into the hybrid anode of solid-state lithium batteries substantially elevates their stability and electrochemical performance. This approach ensures consistent lithium deposition and removal, mitigating dendrite growth and the accumulation of inactive lithium. The findings from this investigation hold significant value in elevating the reversibility and energy density of lithium-ion batteries, thereby making noteworthy contributions to the advancement of more efficient energy storage systems.

Keywords: MCMB, lithium metal, hybrid anode, silver nanoparticle, cycling stability

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Authors: Alok Raghav, Jamal Ahmad

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Background: Serum albumin glycation and advanced glycation end products (AGE) formation correlates in diabetes and its associated complications. Extensive modified human serum albumin is used to study the biochemical, electrochemical and functional properties in hyperglycemic environment with relevance to diabetes. We evaluate Spectroscopic, side chain modifications, amino acid analysis, biochemical and functional group properties in four glucose modified samples. Methods: A series four human serum albumin samples modified with glucose was characterized in terms of amino acid analysis, spectroscopic properties and side chain modifications. The diagnostic technique employed incorporates UV Spectroscopy, Fluorescence Spectroscopy, biochemical assays for side chain modifications, amino acid estimations. Conclusion: Glucose modified human serum albumin confers AGE formation causes biochemical and functional property that depend on the reactivity of glucose and its concentration used for in-vitro glycation. A biochemical and functional characterization of modified albumin in-vitro produced AGE product that will be useful to interpret the complications and pathophysiological significance in diabetes.

Keywords: glycation, diabetes, human serum albumin, biochemical and electrochemical characterization

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Authors: Sharda Nara, Bansi Dhar Malhotra

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Investigation of the vitamins as an electron transfer mediator could significantly assist in merging the area of tissue engineering and electronics required for the implantable therapeutic devices. The present study report that the molecules of folic acid released by Providencia rettgeri via fermentation route under the anoxic condition of the microbial fuel cell (MFC) exhibit characteristic electrochemical and optical properties, as indicated by absorption spectroscopy, photoluminescence (PL), and cyclic voltammetry studies. The absorption spectroscopy has depicted an absorption peak at 263 nm with a small bulge around 293 nm on day two of bacterial culture, whereas an additional peak was observed at 365 nm on the twentieth day. Furthermore, the PL spectra has indicated that the maximum emission occurred at various wavelengths 420, 425, 440, and 445 nm when excited by 310, 325, 350, and 365 nm. The change of emission spectra with varying excitation wavelength might be indicating the presence of tunable optical bands in the folic acid molecules co-related with the redox activity of the molecules. The results of cyclic voltammetry studies revealed that the oxidation and reduction occurred at 0.25V and 0.12V, respectively, indicating the electrochemical behavior of the folic acid. This could be inferred that the released folic acid molecules in a MFC might undergo inter as well as intra molecular electron transfer forming different intermediate states while transferring electrons to the electrode surface. Synchronization of electrochemical and optical properties of folic acid molecules could be potentially promising for the designing of electroactive scaffold and biocompatible conductive surface for the applications of tissue engineering and biofuel cells, respectively.

Keywords: biofuel cell, electroactivity, folic acid, tissue engineering

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Authors: M. Kowalski, M. Brodowski, K. Dziabowska, E. Czaczyk, W. Bialobrzeska, N. Malinowska, S. Zoledowska, R. Bogdanowicz, D. Nidzworski

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Boron-doped-carbon nanowall (BCNW) electrodes are recently in much interest among scientists. BCNWs are good candidates for biosensor purposes as they possess interesting electrochemical characteristics like a wide potential range and the low difference between redox peaks. Moreover, from technical parameters, they are mechanically resistant and very tough. The production process of the microwave plasma-enhanced chemical vapor deposition (MPECVD) allows boron to build into the structure of the diamond being formed. The effect is the formation of flat, long structures with sharp ends. The potential of these electrodes was checked in the biosensing field. The procedure of simple carbon electrodes modification by antibodies was adopted to BCNW for specific antigen recognition. Surface protein D deriving from H. influenzae pathogenic bacteria was chosen as a target analyte. The electrode was first modified with the aminobenzoic acid diazonium salt by electrografting (electrochemical reduction), next anti-protein D antibodies were linked via 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride/N-hydroxysuccinimide (EDC/NHS) chemistry, and free sites were blocked by BSA. Cyclic voltammetry measurements confirmed the proper electrode modification. Electrochemical impedance spectroscopy records indicated protein detection. The sensor was proven to detect protein D in femtograms. This work was supported by the National Centre for Research and Development (NCBR) TECHMATSTRATEG 1/347324/12/NCBR/ 2017.

Keywords: anti-protein D antibodies, boron-doped carbon nanowall, impedance spectroscopy, Haemophilus influenzae.

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Authors: G. Nyongombe, Guy L. Kabongo, B. M. Mothudi, M. S. Dhlamini

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A series of Transition Metals Oxides (TMOs) doped graphene were synthesized and successfully used as supercapacitor electrode materials. The as-synthesized materials exhibited exceptional electrochemical properties owing to the combined properties of its constituents; high surface area and good conductivity were achieved. Several analytical characterization techniques were employed to investigate the morphology, crystal structure atomic arrangement and elemental chemical state in the materials for which scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were conducted, respectively. Moreover, the electrochemical properties of the as-synthesized materials were examined by performing cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) measurements. Furthermore, the effect of doping concentration on the interlayer distance of the graphene materials and the charge transfer resistance are investigated and correlated to the exceptional current density which was multiplied by a factor of ~80 after TMOs doping in graphene. Finally, the resulting high capacitance obtained confirms the contribution of grapheme exceptional electronic conductivity and large surface area on the electrode materials. Such good-performing electrode materials are highly promising for supercapacitors and other energy storage devices.

Keywords: energy density, graphene, supercapacitors, TMOs

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Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky

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The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

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Authors: O. Guellati, A. Harat, F. Djefaflia, N. Habib, A. Nait-Merzoug, J. El Haskouri, D. Momodu, N. Manyala, D. Bégin, M. Guerioune

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We report a facile and low-cost free-template synthesis method was used to synthesize mesoporous smart multifunctional nanohybrids based on Graphene/PANI nanofibers micro/nanostructures with very interesting physic-chemical properties and faradic electrochemical behavior of these products was investigated. These nanohybrid products have been characterized quantitatively and qualitatively using different techniques, such as XRD / FTIR, Raman, XPS spectroscopy, Field Emission SEM and High-Resolution TEM microscopy, BET textural analysis, electrochemical measurements (CV, CD, EIS). Moreover, the electrochemical measurements performed in a 6 M KOH aqueous electrolyte depicted excellent electrochemical performance ascribed to the optimized composition of hydroxides et PANI nanofibers. An exceptionally notable specific capacitance between 800  and 2000 F. g-1 was obtained at 5  mV. s-1 scan rate for these synthesized products depends on the optimized growth conditions. We found much better nanohybrids by reinforcing hydroxides or conduction polymer nanofibers with carbonaceous nanomaterials depicting their potential as suitable materials for energy storage devices.

Keywords: nanohybrid materials, conducting polymers, carbonaceous nanomaterials, supercapacitors, energy storage

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Authors: M. H. Belahssen, S. Benramache

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This paper presents corrosion behavior of alloy 42CrMo4 steel nitrided by plasma. Different samples nitrided were tested. The corrosion behavior was evaluated by electrochemical impedance spectroscopy and the tests were carried out in acid chloride solution 1M. The best corrosion protection was observed for nitrided samples. The aim of this work is to compare equivalents circuits corresponding to Nyquist curves simulated and experimental and select who gives best results of impedance parameters with lowest error.

Keywords: pasma nitriding, steel, alloy 42CrMo4, elecrochemistry, corrosion behavior

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Authors: Mohadeseh Seyednezhad, Armin Rajabi, Andanastui Muchtar, Mahendra Rao Somalu

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This work investigates the electrical properties of NiO-SDC/SDC anode sintered at about 1200 ○C for 1h through a relatively new approach, namely the microwave method. Nano powders Sm0.2Ce0.8O1.9 (SDC) and NiO were mixed by using a high-energy ball-mill and subsequent co-pressed at three different compaction pressures 200, 300 and 400 MPa. The novelty of this study consists in the effect of compaction pressure on the electrochemical performance of Ni-SDC/SDC anode, with no binder used between layers. The electrical behavior of the prepared anode has been studied by electrochemical impedance spectra (EIS) in controlled atmospheres, operating at high temperatures (600-800 °C).

Keywords: sintering, fuel cell, electrical conductivity, nanostructures, impedance spectroscopy, ceramics

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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: V. Pérez-Herranz, C. González-Buch, E. M. Ortega, S. Mestre

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In this work new macroporous Ni electrodes modified with Au nanoparticles for hydrogen production have been developed. The supporting macroporous Ni electrodes have been obtained by means of the electrodeposition at high current densities. Then, the Au nanoparticles were synthesized and added to the electrode surface. The electrocatalytic behaviour of the developed electrocatalysts was studied by means of pseudo-steady-state polarization curves, electrochemical impedance spectroscopy (EIS) and hydrogen discharge curves. The size of the Au synthetized nanoparticles shows a monomodal distribution, with a very sharp band between 10 and 50 nm. The characteristic parameters d10, d50 and d90 were 14, 20 and 31 nm respectively. From Tafel polarization data has been concluded that the Au nanoparticles improve the catalytic activity of the developed electrodes towards the HER respect to the macroporous Ni electrodes. EIS permits to obtain the electrochemically active area by means of the roughness factor value. All the developed electrodes show roughness factor values in the same order of magnitude. From the activation energy results it can be concluded that the Au nanoparticles improve the intrinsic catalytic activity of the macroporous Ni electrodes.

Keywords: Au nano particles, hydrogen evolution reaction, porous Ni electrodes, electrochemical impedance spectroscopy

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Authors: Ahmed A. Farag, M. A. Hgazy

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The influence of three Schiff bases (SB-I, SB-II, and SB-III) on the corrosion of carbon steel in 0.5 M H2SO4 solution was studied by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. The inhibition efficiency increases with the concentration of the Schiff bases and follow the trend: SB-III > SB-II > SB-I. Tafel polarization measurements revealed that the three tested inhibitors function as anodic inhibitors. The thermodynamic parameters Kads and ΔGºads are calculated and discussed. The Langmuir isotherm equation was found to provide an accurate description of the adsorption behaviour of the investigated Schiff bases. Depending on the results, the inhibitive mechanism was proposed.

Keywords: Schiff bases, corrosion inhibitors, EIS, adsorption

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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: Parvin Samadi Pakchin, Reza Saber, Hossein Ghanbari, Yadollah Omidi

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Ovarian cancer is one of the leading cause of mortality among the gynecological malignancies, and it remains the one of the most prevalent cancer in females worldwide. Tumor markers are biochemical molecules in blood or tissues which can indicates cancers occurrence in the human body. So, the sensitive and specific detection of cancer markers typically recruited for diagnosing and evaluating cancers. Recently extensive research efforts are underway to achieve a simple, inexpensive and accurate device for detection of cancer biomarkers. Compared with conventional immunoassay techniques, electrochemical immunosensors are of great interest, because they are specific, simple, inexpensive, easy to handling and miniaturization. Moreover, in the past decade nanotechnology has played a crucial role in the development of biosensors. In this study, a signal-off electrochemical immunosensor for the detection of CA125 antigen has been developed using chitosan-gold nanoparticles (CS-AuNP) and multi-wall carbon nanotubes (MWCNT) composites. Toluidine blue (TB) is used as redox probe which is immobilized on the electrode surface. CS-AuNP is synthesized by a simple one step method that HAuCl4 is reduced by NH2 groups of chitosan. The CS-AuNP-MWCNT modified electrode has shown excellent electrochemical performance compared with bare Au electrode. MWCNTs and AuNPs increased electrochemical conductivity and accelerate electrons transfer between solution and electrode surface while excessive amine groups on chitosan lead to the effective loading of the biological material (CA125 antibody) and TB on the electrode surface. The electrochemical, immobilization and sensing properties CS-AuNP-MWCNT-TB modified electrodes are characterized by cyclic voltammetry, electrochemical impedance spectroscopy, differential pulse voltammetry and square wave voltammetry with Fe(CN)63−/4−as an electrochemical redox indicator.

Keywords: signal-off electrochemical biosensor, CA125, ovarian cancer, chitosan-gold nanoparticles

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Authors: M. Dekmouche, M. Hadjada, Z. Rahmani, M. Saidi

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The effect of iodide ions on the corrosion inhibition of mild steel in 20% sulfuric acid in the presence of 3-méthylthio-5-p-méthoxyphényl-1,2-dithiolylium against anion (I-) A1 synthesized in our laboratory,was studied by different electrochemical techniques such as electrochemical impedance spectroscopy, potentiodynamic polarization. The obtained results showed that A1 effectively reduces the corrosion rate of steel. The adsorption of 3-méthylthio-5-p-méthoxyphényl-1,2-dithiolylium against anion (I-) followed Langmuir and temkin adsorption isotherm.

Keywords: steel XC52, corrosion, inhibition, 3-méthylthio-5-p-méthoxyphényl-1, 2-dithiolylium against anion (I-) , sulfuric acid

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Authors: Abdi Djamila, Haffar Hichem

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The poly methylene bleu (PMB) has been successfully electro deposited on fluorine doped tin oxide (FTO) conducting glass as substrate. Its optical, electrical and photoelectrochemical characterizations have been carried out in order to show the performances of such polymer. The deposited film shows a good electric conductivity which is well confirmed by the low gap value determinated optically by UV–vis spectroscopy. Like all polymers the PMB presents an absorption difference in the visible range function of the polarization potential, it is expressed by the strong conjugation at oxidized state but is weakened with leucoform formation at reduced state. The electrochemical analysis of the films permit to show the cyclic voltamperogram with the anodic oxidation and cathodic reduction states of the polymer and to locate the corresponding energy levels HOMO and LUMO of this later. The electrochemical impedance spectroscopy permit to see the conductive character of such film and to calculate important parameters as Rtc and CPE. The study of the photoelectro activity of our polymer shows that under exposure to intermittent light source this later exhibit important photocurrents which enables it to be used in photo organic ells.

Keywords: polymethylene blue, electropolymerization, homo-lumo, photocurrents

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Authors: Okba Belahssen, Lazhar Torchane, Said Benramache, Abdelouahed Chala

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This paper presents corrosion behavior of the plasma-nitrided 32CrMoV13 steel. Different kinds of samples were tested: non-treated, plasma nitrided samples. The structure of layers was determined by X-ray diffraction, while the morphology was observed by scanning electron microscopy (SEM). The corrosion behavior was evaluated by electrochemical techniques (potentiodynamic curves and electrochemical impedance spectroscopy). The corrosion tests were carried out in acid chloride solution (HCl 1M). Experimental results showed that the nitrides ε-Fe2−3N and γ′-Fe4N present in the white layer are nobler than the substrate but may promote, by galvanic effect, a localized corrosion through open porosity. The better corrosion protection was observed for nitrided sample.

Keywords: plasma-nitrided, 32CrMoV13 steel, corrosion, EIS

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

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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

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Authors: Radka Gorejova, Ivana Sisolakova, Jana Shepa, Frederika Chovancova, Renata Orinakova

Abstract:

Diabetes mellitus (DM) is a serious metabolic disease characterized by chronic hyperglycemia. Often, the symptoms are not sufficiently observable at early stages, and so hyperglycemia causes pathological and functional changes before the diagnosis of the DM. Therefore, the development of an electrochemical sensor that will be fast, accurate, and instrumentally undemanding is currently needful. Screen-printed carbon electrodes (SPCEs) can be considered as the most suitable matrix material for insulin sensors because of the small size of the working electrode. It leads to the analyst's volume reduction to only 50 µl for each measurement. The surface of bare SPCE was modified by a combination of chitosan, multi-walled carbon nanotubes (MWCNTs), and zinc nanoparticles (ZnNPs) to obtain better electrocatalytic activity towards insulin oxidation. ZnNPs were electrochemically deposited on the chitosan-MWCNTs/SPCE surface using the pulse deposition method. Thereafter, insulin was determined on the prepared electrode using chronoamperometry and electrochemical impedance spectroscopy (EIS). The chronoamperometric measurement was performed by adding a constant amount of insulin in 0.1 M NaOH and PBS (2 μl) with the concentration of 2 μM, and the current response of the system was monitored after a gradual increase in concentration. Subsequently, the limit of detection (LOD) of the prepared electrode was determined via the Randles-Ševčík equation. The LOD was 0.47 µM. Prepared electrodes were studied also as the impedimetric sensors for insulin determination. Therefore, various insulin concentrations were determined via EIS. Based on the performed measurements, the ZnNPs/chitosan-MWCNTs/SPCE can be considered as a potential candidate for novel electrochemical sensor for insulin determination. Acknowledgments: This work has been supported by the projects Visegradfund project number 22020140, VEGA 1/0095/21 of the Slovak Scientific Grant Agency, and APVV-PP-COVID-20-0036 of the Slovak Research and Development Agency.

Keywords: zinc nanoparticles, insulin, chronoamperometry, electrochemical impedance spectroscopy

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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: Mandlenkosi G. R. Mahlobo, Peter A. Olubambi, Philippe Refait

Abstract:

The aim of this study was to use voltammetry as a method to understand the behaviour 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 the ohmic drop. Voltammetry was finally performed on 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 deduced 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: Sarah Fahad Alajmi, Tamer Ezzat Youssef

Abstract:

Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

Procedia PDF Downloads 126