Search results for: electrochemical determination

Authors: Sergey A. Burikov, Tatiana A. Dolenko, Kirill A. Gushchin, Sergey A. Dolenko

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The paper presents the results of clusterization by Kohonen self-organizing maps (SOM) applied for analysis of array of Raman spectra of multi-component solutions of inorganic salts, for determination of types of salts present in the solution. It is demonstrated that use of SOM is a promising method for solution of clusterization and classification problems in spectroscopy of multi-component objects, as attributing a pattern to some cluster may be used for recognition of component composition of the object.

Keywords: Kohonen self-organizing maps, clusterization, multi-component solutions, Raman spectroscopy

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Authors: Lawrence I. Onyeji, Girish M. Kale, M. Bijan Kermani

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Corrosion problem which exists in every stage of oil and gas production has been a great challenge to the operators in the industry. The conventional carbon steel with all its inherent advantages has been adjudged susceptible to the aggressive corrosion environment of oilfield. This has aroused increased interest in the use of micro alloyed steels for oil and gas production and transportation. The corrosion behavior of three commercially supplied micro alloyed steels designated as A, B, and C have been investigated with API 5L X65 as reference samples. Electrochemical corrosion tests were conducted in an unbuffered 3.5 wt% NaCl solution saturated with CO₂ at 30 ⁰C for 24 hours. Pre-corrosion analyses revealed that samples A, B and X65 consist of ferrite-pearlite microstructures but with different grain sizes, shapes and distribution whereas sample C has bainitic microstructure with dispersed acicular ferrites. The results of the electrochemical corrosion tests showed that within the experimental conditions, the corrosion rate of the samples can be ranked as CR_(A)< CR_(X65)< CR_(B)< CR_(C). These results are attributed to difference in microstructures of the samples as depicted by ASTM grain size number in accordance with ASTM E112-12 Standard and ferrite-pearlite volume fractions determined by ImageJ Fiji grain size analysis software.

Keywords: carbon dioxide corrosion, corrosion behaviour, micro-alloyed steel, microstructures

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Authors: Z. Khalifa, K. M. Hassan, M. Abdel Azzem

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Potential strategies for deriving useful forms of renewable high density energy from abundant energy stored in carbohydrates is direct conversion of glucose (GLU) to electrical power. A three novel versatile modified electrodes, synthesized by electrochemical polymerization of organic monomers on glassy carbon electrodes (GC), have been developed for biofuel cells results in stable and long-term power production. Electrocatalytic oxidation of glucose in alkaline solution on conducting polymers electrodes modified by incorporation of Ni nanoparticles (NiNPs) onto poly(1,5-aminonaphthalene) (1,5-PDAN), poly(1,8-diaminonaphthalene) (1,8-PDAN) and poly(1-amino-2-methyl-9,10-anthraquinone) (PAMAQ) was investigated. The electrocatalytic oxidation of glucose at NiNPs-modified 1,5-PDAN/GC, 1,8-PDAN/GC and PAMAQ/GC electrodes has been studied using voltammetry technique. The PDAN electrodes show a slight activity in the potential of interest. The prepared NiNPs/PAMAQ/GC catalyst showed a very interesting catalytic activity that was nicely comparable to the NiNPs/1,5-PDAN/GC, NiNPs/1,8-PDAN/GC modified electrodes. In advance, both shows a significant more catalytic activity compared to the reported data for electrodes for glucose electrocatalytic oxidation.

Keywords: biofuel cells, glucose oxidation, electrocatalysis, nanoparticles and modified electrodes

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Authors: Asmaa Mandour, Ramzia El-Bagary, Asmaa El-Zaher, Ehab Elkady

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Background: An UHPLC (ultra high performance liquid chromatography) method for the simultaneous determination of norfloxacin (NOR), metronidazole (MET) and tinidazole (TNZ) using monolithic column is presented. Purpose: The method is considered an environmentally friendly method with relatively low organic composition of the mobile phase. Methods: The chromatographic separation was performed using Phenomenex® Onyex Monolithic C18 (50mmx 20mm) column. An elution program of mobile phase consisted of 0.5% aqueous phosphoric acid : methanol (85:15, v/v). Where elution of all drugs was completed within 3.5 min with 1µL injection volume. The UHPLC method was applied for the stability indication of NOR in the presence of its acid degradation product ND. Results: Retention times were 0.69, 1.19 and 3.23 min for MET, TNZ and NOR, respectively. While ND retention time was 1.06 min. Linearity, accuracy, and precision were acceptable over the concentration range of 5-50µg mL-1for all drugs. Conclusions: The method is simple, sensitive and suitable for the routine quality control and dosage form assay of the three drugs and can also be used for the stability indication of NOR in the presence of its acid degradation product.

Keywords: antibacterial, monolithic cilumn, simultaneous determination, UHPLC

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Authors: Rhea Patel, Madhuri Vinchurkar, Rajul Patkar, Gopal Pranjale, Maryam Shojaei Baghini

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One of the major limitations on food resources worldwide is the deterioration of plant products due to pathogenic infections. Early screening of plants for pathogenic infections can serve as a boon in the Agricultural sector. The standard microbiology techniques has not kept pace with the rapid enumeration and automated methods for bacteria detection. Electrochemical Impedance Spectroscopy (EIS) serves as a label free bio sensing technique to monitor pathogens in real time. The changes in the electrical impedance of a growing bacterial culture can be monitored to detect activity of microorganisms. In this study, we demonstrate development of a gold interdigitated electrode (gold IDE) based impedance biosensor to detect bacterial cells in real on-field crop samples. To calibrate our impedance measurement system, nutrient broth suspended Escherichia coli cells were used. We extended this calibrated protocol to identify the agricultural pathogens in real potato tuber samples. Distinct difference was seen in the impedance recorded for the healthy and infected potato samples. Our results support the potential application of this Impedance based biosensor in Agricultural pathogen detection.

Keywords: agriculture, biosensor, electrochemical impedance spectroscopy, microelectrode, pathogen detection

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Authors: Churamani Pokhrel, C. B. Jha, S. R. Niraula, P. R. Pokharel

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Human identification is one of the most challenging subjects that man has confronted. The determination of adult sex and stature are two of the four key factors (sex, stature, age, and race) in identification of an individual. Craniofacial and odontometric parameters are important tools for forensic anthropologists when it is not possible to apply advanced techniques for identification purposes. The present study provides anthropometric correlation of the parameters with stature and gender and also devises regression formulae for reconstruction of stature. A total of 312 Nepalese students with equal distribution of sex i.e., 156 male and 156 female students of age 18-35 years were taken for the study. Total of 10 parameters were measured (age, sex, stature, head circumference, head length, head breadth, facial height, bi-zygomatic width, mesio-distal canine width and inter-canine distance of both maxilla and mandible). Co-relation and regression analysis was done to find the association between the parameters. All parameters were found to be greater in males than females and each was found to be statistically significant. Out of total 312 samples, the best regressor for the determination of stature was head circumference and mandibular inter-canine width and that for gender was head circumference and right mandibular teeth. The accuracy of prediction was 83%. Regression equations and analysis generated from craniofacial and odontometric parameters can be a supplementary approach for the estimation of stature and gender when extremities are not available.

Keywords: craniofacial, gender, odontometric, stature

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Authors: Anteneh Wodaje Bayeh, Daniel Manaye Kabtamu, Chen-Hao Wang

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As one of the most promising electrochemical energy storage systems, vanadium redox flow batteries (VRFBs) have received increasing attention owing to their attractive features for largescale storage applications. However, their high production cost and relatively low energy efficiency still limit their feasibility. For practical implementation, it is of great interest to improve their efficiency and reduce their cost. One of the key components of VRFBs that can greatly influence the efficiency and final cost is the electrode, which provide the reactions sites for redox couples (VO²⁺/VO₂ + and V²⁺/V³⁺). Carbon-based materials are considered to be the most feasible electrode materials in the VRFB because of their excellent potential in terms of operation range, good permeability, large surface area, and reasonable cost. However, owing to limited electrochemical activity and reversibility and poor wettability due to its hydrophobic properties, the performance of the cell employing carbon-based electrodes remained limited. To address the challenges, we synthesized heteroatom-doped bimetallic oxide grown on the surface of carbon through the one-step approach. When applied to VRFBs, the prepared electrode exhibits significant electrocatalytic effect toward the VO²⁺/VO₂ + and V³⁺/V²⁺ redox reaction compared with that of pristine carbon. It is found that the presence of heteroatom on metal oxide promotes the absorption of vanadium ions. The controlled morphology of bimetallic metal oxide also exposes more active sites for the redox reaction of vanadium ions. Hence, the prepared electrode displays the best electrochemical performance with energy and voltage efficiencies of 74.8% and 78.9%, respectively, which is much higher than those of 59.8% and 63.2% obtained from the pristine carbon at high current density. Moreover, the electrode exhibit durability and stability in an acidic electrolyte during long-term operation for 1000 cycles at the higher current density.

Keywords: VRFB, VO²⁺/VO₂ + and V³⁺/V²⁺ redox couples, graphite felt, heteroatom-doping

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Authors: Shimaa A. Higazy, Mohamed S. Selim, Olfat E. El-Azabawy, Abeer A. Hassan

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We designed novel epoxy/graphitic carbon nitride (g-C₃N₄) nanocomposite materials as suitable surface coatings. g-C₃N₄ nanosheets were facilely prepared and dispersed in the epoxy resin via solution casting. This research focuses on the mechanical and anticorrosion properties of g-C₃N₄ nanofiller reinforced epoxy nanocomposites. The structures, sizes, and morphologies of designed polymeric nanocomposites and nanofillers were elucidated using various techniques such as FT-IR, NMR, FE-TEM, FE-SEM. The developed nanocomposite was applied as a surface coating by air-assisted spray method. The structure-property relationship was studied for different concentrations of nanofiller in the epoxy matrix. The anticorrosive properties were studied via electrochemical experiments, including potentiodynamic polarization, electrochemical impedance, and open-circuit potential analyses, as well as salt spray test. Mechanical durability was assessed by various methods, such as impact, T-bending, and crosscut tests. Surface heterogeneity, elasticity, and corrosion-resistance features are among the merits of developed composite. The highest improvement was achieved with well dispersion of g-C₃N₄ sheets fillers. This fascinating epoxy nanostructured coating provides a promising anticorrosive coatings for a sustainable future environment.

Keywords: epoxy, nanocomposite, surface coating, anticorrosive properties, mechanical durability

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Authors: Kathleen Moyer, Nora Ait Boucherbil, Murtaza Zohair, Janna Eaves-Rathert, Cary Pint

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This study demonstrates the significance of interface engineering in the field of structural energy by being the first case where the performance of the system with the structural battery is greater than the performance of the same system with a battery separate from the system. The benefits of improving the interface in the structural battery were tested by creating carbon fiber composite batteries (and independent graphite electrodes and lithium iron phosphate electrodes) with and without an improved interface. Mechanical data on the structural batteries were collected using tensile tests and electrochemical data was collected using scanning electron microscopy equipment. The full-cell lithium-ion structural batteries had capacity retention of over 80% exceeding 100 cycles with an average energy density of 52 W h kg−1 and a maximum energy density of 58 W h kg−1. Most scientific developments in the field of structural energy have been done with supercapacitors. Most scientific developments with structural batteries have been done where batteries are simply incorporated into the structural element. That method has limited advantages and can create mechanical disadvantages. This study aims to show that a large improvement in structure energy research can be made by improving the interface between the structural device and the battery.

Keywords: composite materials, electrochemical performance, mechanical properties, polymer interface, structural batteries

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Authors: Illyas Md Isa, Maryam Musfirah Che Sobry, Mohamad Syahrizal Ahmad, Nurashikin Abd Azis

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A single-walled carbon nanotube (SWCNT) that has been modified with magnesium layered hydroxide 3-(4-methoxyphenyl)propionic acid nanocomposite was proposed for the determination of uric acid and bisphenol A by square wave voltammetry. The results obtained denote that MLH-MPP nanocomposites enhance the sensitivity of the voltammetry detection responses. The best performance is shown by the modified carbon nanotube paste electrode (CNTPE) with the composition of single-walled carbon nanotube: magnesium layered hydroxide 3-(4-methoxyphenyl)propionic acid nanocomposite at 100:15 (% w/w). The linear range where the sensor works well is within the concentration 1.0 10-7 – 1.0 10-4 and 3.0 10-7 – 1.0 10-4 for uric acid and bisphenol A respectively with the limit of detection of 1.0 10-7 M for both organics. The interferences of uric acid and bisphenol A with other organic were studied and most of them did not interfere. The results shown for each experimental parameter on the proposed CNTPE showed that it has high sensitivity, good selectivity, repeatability and reproducibility. Therefore, the modified CNTPE can be used for the determination of uric acid and bisphenol A in real samples such as blood, plastic bottles and foods.

Keywords: bisphenol A, magnesium layered hydroxide 3-(4-methoxyphenyl)propionic acid nanocomposite, Nanocomposite, uric acid

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Authors: G. Kaur, A. P. Kulkarni, S. Giddey

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Production of fuels and chemicals using renewable energy is a promising way for large-scale energy storage and export. Solid oxide electrolysers (SOEs) integrated with renewable source of energy can produce 'Syngas' H₂/CO from H₂O/CO₂ in the desired ratio for further conversion to liquid fuels. As only a waste CO₂ from industrial and power generation processes is utilized in these processes, this approach is CO₂ neutral compared to using fossil fuel feedstock. In addition, the waste heat from industrial processes or heat from solar thermal concentrators can be effectively utilised in SOEs to further reduce the electrical requirements by up to 30% which boosts overall energy efficiency of the process. In this paper, the electrochemical performance of various novel steam/CO₂ reduction electrodes (cathode) would be presented. The efficiency and lifetime degradation data for single cells and a stack would be presented along with the response of cells to variable electrical load input mimicking the intermittent nature of the renewable energy sources. With such optimisation, newly developed electrodes have been tested for 500+ hrs with Faraday efficiency (electricity to fuel conversion efficiency) up to 95%, and thermal efficiency in excess of 70% based upon energy content of the syngas produced.

Keywords: carbon dioxide, steam conversion, electrochemical system, energy storage, fuel production, renewable energy

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Authors: Simrjit Singh, Neeraj Khare

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In recent years, photo-electrochemical (PEC) water splitting with an aim to generate hydrogen (H₂) as a clean and renewable fuel has been the subject of intense research interests. Ferroelectric semiconductors have been demonstrated to exhibit enhanced PEC properties as these can be polarized with the application of an external electric field resulting in a built-in potential which helps in separating out the photogenerated charge carriers. In addition to this, by changing the polarization direction, the energy band alignment at the electrode/electrolyte interface can be modulated in a way that it can help in the easy transfer of the charge carriers from the electrode to the electrolyte. In this paper, we investigated the photoelectrochemical properties of ferroelectric PVDF/Cu/PVDF-NaNbO₃ PEC cell and demonstrated that PEC properties can be tuned with ferroelectric polarization and piezophototronic effect. Photocurrent density is enhanced from ~0.71 mA/cm² to 1.97 mA/cm² by changing the polarization direction. Furthermore, due to flexibility and piezoelectric properties of PVDF/Cu/PVDF-NaNbO₃ PEC cell, a further ~26% enhancement in the photocurrent is obtained using the piezophototronic effect. A model depicting the modulation of band alignment between PVDF and NaNbO₃ with the electric field is proposed to explain the observed tuning of the PEC properties. Electrochemical Impedance spectroscopy measurements support the validity of the proposed model.

Keywords: electrical tuning, H₂ generation, photoelectrochemical, NaNbO₃

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

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Authors: Nusrat Praween, Krishna Thej Pammi Guru, Palash Kumar Basu

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Designing non-invasive biosensors for cancer diagnosis is essential for developing an affordable and specific tool to measure cancer-related exosome biomarkers. Exosomes, released by healthy as well as cancer cells, contain valuable information about the biomarkers of various diseases, including cancer. Despite the availability of various isolation techniques, ultracentrifugation is the standard technique that is being employed. Post isolation, exosomes are traditionally exposed to detergents for extracting their proteins, which can often lead to protein degradation. Further to this, it is very essential to develop a sensing platform for the quantification of clinically relevant proteins in a wider range to ensure practicality. In this study, exosomes were immobilized on the Au Screen Printed Electrode (SPE) using EDC/NHS chemistry to facilitate binding. After immobilizing the exosomes on the screen-printed electrode (SPE), we investigated the impact of the electric field by applying various voltages to induce exosome lysis and release their contents. The lysed solution was used for sensing TSG101, a crucial biomarker associated with various cancers, using both faradaic and non-faradaic electrochemical impedance spectroscopy (EIS) methods. The results of non-faradaic and faradaic EIS were comparable and showed good consistency, indicating that non-faradaic sensing can be a reliable alternative. Hence, the non-faradaic sensing technique was used for label-free quantification of the TSG101 biomarker. The results were validated using ELISA. Our electrochemical immunosensor demonstrated a consistent response of TSG101 from 125 pg/mL to 8000 pg/mL, with a detection limit of 0.125 pg/mL at room temperature. Additionally, since non-faradic sensing is label-free, the ease of usage and cost of the final sensor developed can be reduced. The proposed immunosensor is capable of detecting the TSG101 protein at low levels in healthy serum with good sensitivity and specificity, making it a promising platform for biomarker detection.

Keywords: biosensor, exosomes isolation on SPE, electric field lysis of exosome, EIS sensing of TSG101

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Authors: Wenjun Zhang, Thao Thi Le, Dongyup Shin, Jong Min Kim

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Electrochemical hydrogen peroxide (H₂O₂) synthesis holds significant promise for decentralized environmental remediation through the electro-Fenton process. However, challenges persist, such as the absence of robust electrocatalysts for the selective two-electron oxygen reduction reaction (2e⁻ ORR) and the high cost and sluggish kinetics of conventional electro-Fenton systems in treating highly concentrated wastewater. This study introduces an efficient water treatment system for removing substantial quantities of organic pollutants using an advanced electro-Fenton system coupled with a high-valent NiO catalyst. By employing a precipitation method involving crystal facet and cation vacancy engineering, a trivalent Ni (Ni³⁺)-rich NiO catalyst with a (111)-domain-exposed crystal facet, named {111}-NivO, was synthesized. This catalyst exhibited a remarkable 96% selectivity and a high mass activity of 59 A g⁻¹ for H₂O₂ production, outperforming all previously reported Ni-based catalysts. Furthermore, an advanced electro-Fenton system, integrated with a flow cell for electrochemical H₂O₂ production, was utilized to achieve 100% removal of 50 ppm bisphenol A (BPA) in 200 mL of wastewater under heavy-duty conditions, reaching a superior rapid degradation rate (4 min, k = 1.125 min⁻¹), approximately 102 times faster than the conventional electro-Fenton system. The hyper-efficiency is attributed to the continuous and appropriate supply of H₂O₂, the provision of O₂, and the timely recycling of the electrolyte under high current density operation. This catalyst also demonstrated a 93% removal of total organic carbon after 2 hours of operation and can be applied for efficient removal of highly concentrated phenol pollutants from aqueous systems, which opens new avenues for wastewater treatment.

Keywords: hydrogen peroxide production, nickel oxides, crystal facet and cation vacancy engineering, wastewater treatment, flow cell, electro-Fenton

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Authors: Gabriel Wosiak, Dyovani Coelho, Evaldo B. Carneiro-Neto, Ernesto C. Pereira, Mauro C. Lopes

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In this work, the theoretical and experimental effects of induced charging currents on fast-scan cyclic voltammetry (FSCV) are investigated. Induced charging currents arise from the effect of ohmic drop in electrochemical systems, which depends on the presence of an uncompensated resistance. They cause the capacitive contribution to the total current to be different from the capacitive current measured in the absence of electroactive species. The paper shows that the induced charging current is relevant when the capacitive current magnitude is close to the total current, even for systems with low time constant. In these situations, the conventional background subtraction method may be inaccurate. A method is developed that separates the faradaic and capacitive currents by using a combination of voltametric experimental data and finite element simulation, by the obtention of a potential-dependent capacitance. The method was tested in a standard electrochemical cell with Platinum ultramicroelectrodes, in different experimental conditions as well in previously reported data in literature. The proposed method allows the real capacitive current to be separated even in situations where the conventional background subtraction method is clearly inappropriate.

Keywords: capacitive current, fast-scan cyclic voltammetry, finite-element method, electroanalysis

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Authors: Youtao Gao, Bingyu Jin, Tanran Zhao, Bo Xu

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The history of satellite navigation can be dated back to the 1960s. From the U.S. Transit system and the Russian Tsikada system to the modern Global Positioning System (GPS) and the Globalnaya Navigatsionnaya Sputnikovaya Sistema (GLONASS), performance of satellite navigation has been greatly improved. Nowadays, the navigation accuracy and coverage of these existing systems have already fully fulfilled the requirement of near-Earth users, but these systems are still beyond the reach of deep space targets. Due to the renewed interest in space exploration, a novel high-precision satellite navigation system is becoming even more important. The increasing demand for such a deep space navigation system has contributed to the emergence of a variety of new constellation architectures, such as the Lunar Global Positioning System. Apart from a Walker constellation which is similar to the one adopted by GPS on Earth, a novel constellation architecture which consists of libration point satellites in the Earth-Moon system is also available to construct the lunar navigation system, which can be called accordingly, the libration point satellite navigation system. The concept of using Earth-Moon libration point satellites for lunar navigation was first proposed by Farquhar and then followed by many other researchers. Moreover, due to the special characteristics of Libration point orbits, an autonomous orbit determination technique, which is called ‘Liaison navigation’, can be adopted by the libration point satellites. Using only scalar satellite-to-satellite tracking data, both the orbits of the user and libration point satellites can be determined autonomously. In this way, the extensive Earth-based tracking measurement can be eliminated, and an autonomous satellite navigation system can be developed for future space exploration missions. The method of state estimate is an unnegligible factor which impacts on the orbit determination accuracy besides type of orbit, initial state accuracy and measurement accuracy. We apply the extended Kalman filter(EKF) and the unscented Kalman filter(UKF) to determinate the orbits of Lagrangian navigation satellites. The autonomous orbit determination errors are compared. The simulation results illustrate that UKF can improve the accuracy and z-axis convergence to some extent.

Keywords: extended Kalman filter, autonomous orbit determination, unscented Kalman filter, navigation constellation

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Authors: Faisal A. Salih

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Verapamil hydrochloride (Ver) is a drug used in medicine for arrythmia, angina and hypertension as a calcium channel blocker. For the quantitative determination of Ver in dosage forms, the HPLC method is most often used. A convenient alternative to the chromatographic method is potentiometry using a Verselective electrode, which does not require expensive equipment, can be used without separation from the matrix components, which significantly reduces the analysis time, and does not use toxic organic solvents, being a "green", "environmentally friendly" technique. It has been established in this study that the rational choice of the membrane plasticizer and the preconditioning and measurement algorithms, which prevent nonexchangeable extraction of Ver into the membrane phase, makes it possible to achieve excellent analytical characteristics of Ver-selective electrodes based on commercially available components. In particular, an electrode with the following membrane composition: PVC (32.8 wt %), ortho-nitrophenyloctyl ether (66.6 wt %), and tetrakis-4-chlorophenylborate (0.6 wt % or 0.01 M) have the lower detection limit 4 × 10−8 M and potential reproducibility 0.15–0.22 mV. Both direct potentiometry (DP) and potentiometric titration (PT) methods can be used for the determination of Ver in tablets and injection solutions. Masses of Ver per average tablet weight determined by the methods of DP and PT for the same set of 10 tablets were (80.4±0.2 and80.7±0.2) mg, respectively. The masses of Ver in solutions for injection, determined by DP for two ampoules from one set, were (5.00±0.015 and 5.004±0.006) mg. In all cases, good reproducibility and excellent correspondence with the declared quantities were observed.

Keywords: verapamil, potentiometry, ion-selective electrode, pharmaceutical analysis

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Authors: Boriana Karamanova, Svetlana Veleva, Luybomir Soserov, Ana Arenillas, Francesco Lufrano, Antonia Stoyanova

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Supercapacitors have received a lot of research attention and are promising energy storage devices due to their high power and long cycle life. In order to developed an advanced device with significant capacity for storing charge and cheap carbon materials, efforts must focus not only on improving synthesis by controlling the morphology and pore size but also on improving electrode-electrolyte compatibility of the resulting systems. The present study examines the relationship between the surface chemistry of two activated carbon xerogels, the electrolyte type, and the electrochemical properties of supercapacitors. Activated carbon xerogels were prepared by varying the initial pH of the resorcinol-formaldehyde aqueous solution. The materials produced are physicochemical characterized by DTA/TGA, porous characterization, and SEM analysis. The carbon xerogel based electrodes were prepared by spreading over glass plate a slurry containing the carbon gel, graphite, and poly vinylidene difluoride (PVDF) binder. The layer formed was dried consecutively at different temperatures and then detached by water. After, the layer was dried again to improve its mechanical stability. The developed electrode materials and the Aquivion® E87-05S membrane (Solvay Specialty Polymers), socked in Na2SO4 as a polymer electrolyte, were used to assembly the solid-state supercapacitor. Symmetric supercapacitor cells composed by same electrodes and 1 M KOH electrolytes are also assembled and tested for comparison. The supercapacitor performances are verified by different electrochemical methods - cyclic voltammetry, galvanostatic charge/discharge measurements, electrochemical impedance spectroscopy, and long-term durability tests in neutral and alkaline electrolytes. Specific capacitances, energy, and power density, energy efficiencies, and durability were compared into studied supercapacitors. Ex-situ physicochemical analyses on the synthesized materials have also been performed, which provide information about chemical and structural changes in the electrode morphology during charge / discharge durability tests. They are discussed on the basis of electrode-electrolyte interaction. The obtained correlations could be of significance in order to design sustainable solid-state supercapacitors with high power and energy density. Acknowledgement: This research is funded by the Ministry of Education and Science of Bulgaria under the National Program "European Scientific Networks" (Agreement D01-286 / 07.10.2020, D01-78/30.03.2021). Authors gratefully acknowledge.

Keywords: carbon xerogel, electrochemical tests, neutral and alkaline electrolytes, supercapacitors

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Authors: Feixiong Chen, Naoufel Haddour, Marie Frenea-Robin, Yves MéRieux, Yann Chevolot, Virginie Monnier

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Neonatal thrombopenia occurs when the mother generates antibodies against her baby’s platelet antigens. It is particularly critical for newborns because it can cause coagulation troubles leading to intracranial hemorrhage. In this case, diagnosis must be done quickly to make platelets transfusion immediately after birth. Before transfusion, platelet antigens must be tested carefully to avoid rejection. The majority of thrombopenia (95 %) are caused by antibodies directed against Human Platelet Antigen 1a (HPA-1a) or 5b (HPA-5b). The common method for antigen platelets detection is polymerase chain reaction allowing for identification of gene sequence. However, it is expensive, time-consuming and requires significant blood volume which is not suitable for newborns. We propose to develop a point-of-care device based on double functionalized magnetic colloids with 1) antibodies specific to antigen platelets and 2) highly sensitive electroactive molecules in order to be detected by an electrochemical microsensor. These magnetic colloids will be used first to isolate platelets from other blood components, then to capture specifically platelets bearing HPA-1a and HPA-5b antigens and finally to attract them close to sensor working electrode for improved electrochemical signal. The expected advantages are an assay time lower than 20 min starting from blood volume smaller than 100 µL. Our functionalization procedure based on amine dendrimers and NHS-ester modification of initial carboxyl colloids will be presented. Functionalization efficiency was evaluated by colorimetric titration of surface chemical groups, zeta potential measurements, infrared spectroscopy, fluorescence scanning and cyclic voltammetry. Our results showed that electroactive molecules and antibodies can be immobilized successfully onto magnetic colloids. Application of a magnetic field onto working electrode increased the detected electrochemical signal. Magnetic colloids were able to capture specific purified antigens extracted from platelets.

Keywords: Magnetic Nanoparticles , Electroactive Molecules, Antibody, Platelet

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Authors: Cumhur Cansever, Selcuk Er

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There is an increasing cooperation and interaction between the military logistic systems and civil organizations operating in today's market. While the scope and functions of civilian logistics have different characteristics, military logistics tries to import some applications that are conducted by private sectors successfully. Also, at this point, the determination of the optimal point of integration and interaction between civilian and military logistics has emerged as a key issue. In this study, the mutual effects between military and civilian logistics and their most common integration areas, (Supply Chain Management (SCM), Integrated Logistics Support (ILS) and Outsourcing) will be examined with risk analysis and determination of basic skills evaluation methods for determining the optimum point in the integration.

Keywords: core competency, integrated logistics support, outsourcing, supply chain management

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Authors: Özkan Özgenç, Serdar Hacisalihoğlu, Murat Yanik

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History has shown that quantitative and qualitative supremacy in terms of military and economic power has been inadequate to reach the desired results. In addition, public support has been a crucial requirement for the success of the any struggle. As a leader seeking ways for the independence of the country, Ataturk comprehended that the only solution was possible with the help of public will and determination. Ataturk needed an impeccable communication strategy to combine efforts by establishing a united notion and action; to convince the world and Turkish nation of the legitimacy and sacredness of Independence struggle; and to show the resolution and determination of Turkish nation against the invaders. To emancipate the Turkish nation, Ataturk shaped the nation's emotions, ideas, and behaviors by using the most appropriate tools at the best time and place since the start of Independence War in May 19, 1919.

Keywords: Atatürk, Turkish independence struggle, strategic communication, independence war

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Authors: A. N. Fouda

Abstract:

A novel well identified hexagonal graphene oxide (GO) nano-sheets were synthesized using modified Hummer method. Low temperature thermal reduction at 350°C in air ambient was performed. After thermal reduction, typical few layers of thermal reduced GO (TRGO) with dimension of few hundreds nanometers were observed using high resolution transmission electron microscopy (HRTEM). GO has a lot of structure models due to variation of the preparation process. Determining the atomic structure of GO is essential for a better understanding of its fundamental properties and for realization of the future technological applications. Structural characterization was identified by x-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR) measurements. A comparison between exper- imental and theoretical IR spectrum were done to confirm the match between experimentally and theoretically proposed GO structure. Partial overlap of the experimental IR spectrum with the theoretical IR was confirmed. The electrochemical properties of TRGO nano-sheets as electrode materials for supercapacitors were investigated by cyclic voltammetry and electrochemical impedance spectroscopy (EIS) measurements. An enhancement in supercapacitance after reduction was confirmed and the area of the CV curve for the TRGO electrode is larger than those for the GO electrode indicating higher specific capacitance which is promising in super-capacitor applications

Keywords: hexagonal graphene oxide, thermal reduction, cyclic voltammetry

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Authors: Azeez O. Idris, Benjamin O. Orimolade, Potlako J. Mafa, Alex T. Kuvarega, Usisipho Feleni, Bhekie B. Mamba

Abstract:

We report a simple and cheaper method for the electrochemical detection of Se(IV) using carbon nanodots (CNDTs) prepared from oat. The carbon nanodots were synthesised by green and facile approach and characterised using scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. The CNDT was used to fabricate an electrochemical sensor for the quantification of Se(IV) in water. The modification of glassy carbon electrode (GCE) with carbon nanodots led to an increase in the electroactive surface area of the electrode, which enhances the redox current peak of [Fe(CN)₆]₃₋/₄‒ in comparison to the bare GCE. Using the square wave voltammetry, the detection limit and quantification limit of 0.05 and 0.167 ppb were obtained under the optimised parameters using deposition potential of -200 mV, 0.1 M HNO₃ electrolyte, electrodeposition time of 60 s, and pH 1. The results further revealed that the GCE-CNDT was not susceptible to many interfering cations except Cu(II) and Pb(II), and Fe(II). The sensor fabrication involves a one-step electrode modification and was used to detect Se(IV) in a real water sample, and the result obtained is in agreement with the inductively coupled plasma technique. Overall, the electrode offers a cheap, fast, and sensitive way of detecting selenium in environmental matrices.

Keywords: carbon nanodots, square wave voltammetry, nanomaterials, selenium, sensor

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Authors: H. Beisch, J. Marx, S. Garlof, R. Shvets, I. I. Grygorchak, A. Kityk, B. Fiedler

Abstract:

Carbon materials, especially three-dimensional carbon foams, show very high potential in the application as electrode material for energy storage systems such as batteries and supercapacitors with unique fast charging and discharging times. Regarding their high specific surface areas (SSA) high specific capacities can be reached. Globugraphite is a newly developed carbon foam with an interconnected globular carbon morphology. Especially, this foam has a statistically distributed hierarchical pore structure resulting from the manufacturing process based on sintered ceramic templates which are synthetized during a final chemical vapor deposition (CVD) process. For morphology characterization scanning electron (SEM) and transmission electron microscopy (TEM) is used. In addition, the SSA is carried out by nitrogen adsorption combined with the Brunauer–Emmett–Teller (BET) theory. Electrochemical measurements in organic and inorganic electrolyte provide high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. All values are summarized in a Ragone Diagram. Finally, power densities up to 833 W/kg and energy densities up to 48 Wh/kg could be achieved. The corresponding SSA is between 376 m²/g and 859 m²/g. For organic electrolyte a specific capacity of 71 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, CVD process, electron microscopy, Ragone diagram

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Authors: Hamide Aydin, Banu Karaman, Ayhan Bozkurt, Umran Kurtan

Abstract:

Recently, Proton Conducting Gel Polymer Electrolytes (GPEs) have drawn much attention in supercapacitor applications due to their physical and electrochemical characteristics and stability conditions for low temperatures. In this research, PVA-H2SO4-H3BO3 GPE has been used for electric-double layer capacitor (EDLCs) application, in which electrospun free-standing carbon nanofibers are used as electrodes. Introduced PVA-H2SO4-H3BO3 GPE behaves as both separator and the electrolyte in the supercapacitor. Symmetric Swagelok cells including GPEs were assembled via using two electrode arrangements and the electrochemical properties were searched. Electrochemical performance studies demonstrated that PVA-H2SO4-H3BO3 GPE had a maximum specific capacitance (Cs) of 134 F g-1 and showed great capacitance retention (%100) after 1000 charge/discharge cycles. Furthermore, PVA-H2SO4-H3BO3 GPE yielded an energy density of 67 Wh kg-1 with a corresponding power density of 1000 W kg-1 at a current density of 1 A g-1. PVA-H2SO4 based polymer electrolyte was produced according to following procedure; Firstly, 1 g of commercial PVA was dissolved in distilled water at 90°C and stirred until getting transparent solution. This was followed by addition of the diluted H2SO4 (1 g of H2SO4 in a distilled water) to the solution to obtain PVA-H2SO4. PVA-H2SO4-H3BO3 based polymer electrolyte was produced by dissolving H3BO3 in hot distilled water and then inserted into the PVA-H2SO4 solution. The mole fraction was arranged to ¼ of the PVA repeating unit. After the stirring 2 h at RT, gel polymer electrolytes were obtained. The final electrolytes for supercapacitor testing included 20% of water in weight. Several blending combinations of PVA/H2SO4 and H3BO3 were studied to observe the optimized combination in terms of conductivity as well as electrolyte stability. As the amount of boric acid increased in the matrix, excess sulfuric acid was excluded due to cross linking, especially at lower solvent content. This resulted in the reduction of proton conductivity. Therefore, the mole fraction of H3BO3 was chosen as ¼ of PVA repeating unit. Within this optimized limits, the polymer electrolytes showed better conductivities as well as stability.

Keywords: electrical double layer capacitor, energy density, gel polymer electrolyte, ultracapacitor

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Authors: Karel Borovec, Jerzy Gorecki, Tadeas Ochodek

Abstract:

Combustion of solid fuels is one of the main sources of mercury in the environment. To reduce the amount of mercury emitted to the atmosphere, it is necessary to modify or optimize old purification technologies or introduce the new ones. Effective reduction of mercury level in the flue gas requires the use of speciation systems for mercury form determination. This paper describes tests and provides comparison of two industrial portable and continuous systems for mercury speciation in the flue gas: Durag HM-1400 TRX with a speciation module and the Portable Continuous Mercury Speciation System based on the SGM-8 mercury speciation set, made by Nippon Instruments Corporation. Additionally, the paper describes a few analytical problems that were encountered during a two-year period of using the systems.

Keywords: continuous measurement, flue gas, mercury determination, speciation

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Authors: Joanna Cabaj, Sylwia Baluta, Karol Malecha

Abstract:

Catecholamines are vital neurotransmitters that mediate a variety of central nervous system functions, such as motor control, cognition, emotion, memory processing, and endocrine modulation. Dysfunctions in catecholamine neurotransmission are induced in some neurologic and neuropsychiatric diseases. Changeable neurotransmitters level in biological fluids can be a marker of several neurological disorders. Because of its significance in analytical techniques and diagnostics, sensitive and selective detection of neurotransmitters is increasingly attracting a lot of attention in different areas of bio-analysis or biomedical research. Recently, optical techniques for the detection of catecholamines have attracted interests due to their reasonable cost, convenient control, as well as maneuverability in biological environments. Nevertheless, with the observed need for a sensitive and selective catecholamines sensor, the development of a convenient method for this neurotransmitter is still at its basic level. The manipulation of nanostructured materials in conjunction with biological molecules has led to the development of a new class of hybrid-modified enzymatic sensors in which both enhancement of charge transport and biological activity preservation may be obtained. Immobilization of biomaterials on electrode surfaces is the crucial step in fabricating electrochemical as well as optical biosensors and bioelectronic devices. Continuing systematic investigation in manufacturing of enzyme–conducting sensitive systems, here is presented a convenient fluorescence as well as electrochemical sensing strategy for catecholamines detection.

Keywords: biosensors, catecholamines, fluorescence, enzymes

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Authors: Snehal L. Kadam, Shriniwas B. Kulkarni

Abstract:

Flexible electrode material with high surface area and good electrochemical properties is the current trend captivating the researchers across globe for application in the next generation energy storage field. In the present work, crumpled sheet like reduced graphene oxide grown on carbon cloth by the hydrothermal method with a series of different deposition temperatures at fixed time. The influence of the deposition temperature on the structural, morphological, optical and supercapacitive properties of the electrode material was investigated by XRD, RAMAN, XPS, TEM, FE-SEM, UV-VISIBLE and electrochemical characterization techniques.The results show that the hydrothermally synthesized reduced graphene oxide on carbon cloth has sheet like mesoporous structure. The reduced graphene oxide material at 160°C exhibits the best supercapacitor performance, with a specific capacitance of 443 F/g at scan rate 5mV/sec. Moreover, stability studies show 97% capacitance retention over 1000 CV cycles. This result shows that hydrothermally synthesized RGO on carbon cloth is the potential electrode material and would be used in the next-generation wearable energy storage systems. The detailed analysis and results will be presented at the conference.

Keywords: graphene oxide, reduced graphene oxide, carbon cloth, deposition temperature, supercapacitor

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Authors: Min Yu, Olivier T. Picot, Theo Graves Saunders, Ivo Dlouhy, Amit Mahajan, Michael J. Reece

Abstract:

Graphene was successfully introduced into a polymer-derived silicon oxycarbide (SiOC) matrix by phase transfer of graphene oxide (GO) from an aqueous (GO dispersed in water) to an organic phase (copolymer as SiOC precursor in diethyl ether). With GO concentrations increasing up to 2 vol%, graphene-containing flakes self-assembled into a lamellar structure in the matrix leading to composite with the anisotropic property. Spark plasma sintering (SPS) was applied to densify the composites with four different GO concentrations (0, 0.5, 1 and 2 vol%) up to ~2.3 g/cm3. The fracture toughness of SiOC-2 vol% GO composites was significantly increased by ~91% (from 0.70 to 1.34 MPa·m¹/²), at the expense of a decrease in the flexural strength (from 85MPa to 55MPa), compared to SiOC-0 vol% GO composites. Moreover, the electrical conductivity in the perpendicular direction (σ┴=3×10⁻¹ S/cm) in SiOC-2 vol% GO composite was two orders of magnitude higher than the parallel direction (σ║=4.7×10⁻³ S/cm) owing to the self-assembled lamellar structure of graphene in the SiOC matrix. The composites exhibited increased electrical conductivity (σ┴) from 8.4×10⁻³ to 3×10⁻¹ S/cm, with the increasing GO content from 0.5 to 2 vol%. The SiOC-2 vol% GO composites further showed the better electrochemical performance of oxygen reduction reaction (ORR) than pure graphene, exhibiting a similar onset potential (~0.75V vs. RHE) and more positive half-wave potential (~0.6V vs. RHE).

Keywords: composite, fracture toughness, flexural strength, electrical conductivity, electrochemical performance

Procedia PDF Downloads 166