Search results for: advanced electrochemical oxidation

Authors: Fredrick O. Okumu, Mangaka C. Matoetoe

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

Keywords: characterization, core-shell, electrochemical, nanoparticles

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Authors: Ramon Alberto Paredes Camacho, Li Lu

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Sustainable batteries are possible through the development of cheaper and greener alternatives whose most feasible option is epitomized by Sodium-Ion Batteries (SIB). Na₃V₂(PO₄)₂F₃ (NVPF) an important member of the Na-superionic-conductor (NASICON) materials, has recently been in the spotlight due to its interesting electrochemical properties when used as cathode namely, high specific capacity of 128 mA h g-¹, high energy density of 507 W h Kg-¹, increased working potential at which vanadium redox couples can be activated (with an average value around 3.9 V), and small volume variation of less than 2%. These traits grant NVPF an excellent perspective as a cathode material for the next generation of sodium batteries. Unfortunately, because of its low inherent electrical conductivity and a high energy barrier that impedes the mobilization of all the available Na ions per formula, the overall electrochemical performance suffers substantial degradation, finally obstructing its industrial use. Many approaches have been developed to remediate these issues where nanostructural design, carbon coating, and ion doping are the most effective ones. This investigation is focused on enhancing the electrochemical response of NVPF by doping metal ions in the crystal lattice, substituting vanadium atoms. A facile sol-gel process is employed, with citric acid as the chelator and the carbon source. The optimized conditions circumvent fluorine sublimation, ratifying the material’s purity. One of the reasons behind the large ionic improvement is the attraction of extra Na ions into the crystalline structure due to a charge imbalance produced by the valence of the doped ions (+2), which is lower than the one of vanadium (+3). Superior stability (higher than 90% at a current density of 20C) and capacity retention at an extremely high current density of 50C are demonstrated by our doped NVPF. This material continues to retain high capacity values at low and high temperatures. In addition, full cell NVPF//Hard Carbon shows capacity values and high stability at -20 and 60ºC. Our doping strategy proves to significantly increase the ionic and electronic conductivity of NVPF even at extreme conditions, delivering outstanding electrochemical performance and paving the way for advanced high-potential cathode materials.

Keywords: sodium-ion batteries, cathode materials, NASICON, Na3V2(PO4)2F3, Ion doping

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

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

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

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Authors: Łukasz Mazur, Kamil Domaradzki, Bartosz Kamecki, Justyna Ignaczak, Sebastian Molin, Aleksander Gil, Tomasz Brylewski

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The rising global power consumption necessitates the development of new energy storage solutions. Prospective technologies include solid oxide electrolyzer cells (SOECs), which convert surplus electrical energy into hydrogen. An electrolyzer cell consists of a porous anode, and cathode, and a dense electrolyte. Power output is increased by connecting cells into stacks using interconnects. Interconnects are currently made from high-chromium ferritic steels – for example, Crofer 22 APU – which exhibit high oxidation resistance and a thermal expansion coefficient that is similar to that of electrode materials. These materials have one disadvantage – their area-specific resistance (ASR) gradually increases due to the formation of a Cr₂O₃ scale on their surface as a result of oxidation. The chromia in the scale also reacts with the water vapor present in the reaction media, forming volatile chromium oxyhydroxides, which in turn react with electrode materials and cause their deterioration. The electrochemical efficiency of SOECs thus decreases. To mitigate this, the interconnect surface can be modified with protective-conducting coatings of spinel or other materials. The high prices of SOEC components -especially the Crofer 22 APU- have prevented their widespread adoption. More inexpensive counterparts, therefore, need to be found, and their properties need to be enhanced to make them viable. Candidates include the Nirosta 4016/1,4016 low-chromium ferritic steel with a chromium content of just 16.3 wt%. This steel's resistance to high-temperature oxidation was improved by depositing Gd₂O₃ nanoparticles on its surface via either dip coating or electrolysis. Modification with CeO₂ or Ce₀.₉Y₀.₁O₂ nanoparticles deposited by means of spray pyrolysis was also tested. These methods were selected because of their low cost and simplicity of application. The aim of this study was to investigate the oxidation kinetics of Nirosta 4016/1,4016 modified using the afore-mentioned methods and to subsequently measure the obtained samples' ASR. The samples were oxidized for 100 h in the air as well as air/H₂O and Ar/H₂/H₂O mixtures at 1073 K. Such conditions reflect those found in the anode and cathode operating space during real-life use of SOECs. Phase and chemical composition and the microstructure of oxidation products were determined using XRD and SEM-EDS. ASR was measured over the range of 623-1073 K using a four-point, two-probe DC technique. The results indicate that the applied nanoparticles improve the oxidation resistance and electrical properties of the studied layered systems. The properties of individual systems varied significantly depending on the applied reaction medium. Gd₂O₃ nanoparticles improved oxidation resistance to a greater degree than either CeO₂ or Ce₀.₉Y₀.₁O₂ nanoparticles. On the other hand, the cerium-containing nanoparticles improved electrical properties regardless of the reaction medium. The ASR values of all surface-modified steel samples were below the 0.1 Ω.cm² threshold set for interconnect materials, which was exceeded in the case of the unmodified reference sample. It can be concluded that the applied modifications increased the oxidation resistance of Nirosta 4016/1.4016 to a level that allows its use as SOEC interconnect material. Acknowledgments: Funding of Research project supported by program "Excellence initiative – research university" for the AGH University of Krakow" is gratefully acknowledged (TB).

Keywords: cerium oxide, ferritic stainless steel, gadolinium oxide, interconnect, SOEC

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Authors: Ruchi Jain, Chinnakonda S. Gopinath

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The CO oxidation is a primary reaction in heterogeneous catalysis due to its potential to overcome the air pollution caused by various reasons. Indeed, in the study of sustainable catalysis, the role played by water is very important. The present work is focused on studying the effect of moisture on the sustainability of Co3O4 NR catalyst for CO oxidation reaction at ambient temperature. The catalytic activity, electronic structure and the mechanistic aspects of spinel Co3O4 nanorod surfaces have been explored in dry and wet atmosphere by near-ambient pressure photoelectron spectroscopic techniques (NAP-PES) with conventional x-ray (Al kα) and ultraviolet sources (He-I).Comparative NAPPES studies have been employed to understand the elucidation of the catalytic reaction pathway and the evolution of various surface species. The presence of water with CO+O2 plummet the catalytic activity due to the change in electronic nature from predominantly oxidic (without water in the feed) to few intermediates covered Co3O4 surface. However, ≥ 375 K Co3O4 surface recovers and regain oxidation activity, at least partially, even in the presence of water. Above mentioned observations are fully supported by the changes observed in the work function of Co3O4 in the presence of wet (H2O+CO+O2) compared to dry (CO+O2) conditions. Various type of surface species, such as CO(ads), carbonate, formate, are found to be on the catalyst surface depending on the reaction conditions. Under dry condition, CO couples with labile O atoms to form CO2, however under wet conditions it also interacts with surface OH groups results in the formation carbonate and formate intermediate. The carbonate acts at reaction inhibitor at room temperature, however proves as active intermediate at temperature 375 K or above. On the other hand, formate has proved to be reaction spectator due to its high stability. The intrinsic role of these species to suppress the oxidation has been demonstrated through a possible reaction mechanism under different reaction conditions.

Keywords: heterogeneous catalysis, surface chemistry, photoelectron spectroscopy, ambient oxidation

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Authors: Yaling Gou, Sucai Yang, Pengwei Qiao

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Integrated chemical-biological treatment is an attractive alternative to remove polycyclic aromatic hydrocarbons (PAHs) from contaminated soil; wherein indigenous bacteria is the key factor for the biodegradation of residual PAHs concentrations after the application of chemical oxidation. However, the systematical study on the impact of persulfate (PS) oxidation on indigenous bacteria as well as PAHs removal is still scarce. In this study, the influences of different PS dosages (1%, 3%, 6%, and 10% [w/w]), as well as various activation methods (native iron, H2O2, alkaline, ferrous iron, and heat) on PAHs removal and indigenous bacteria in highly contaminated aged soil were investigated. Apparent degradation of PAHs in the soil treated with PS oxidation was observed, and the removal efficiency of total PAHs in the soil ranged from 38.28% to 79.97%. The removal efficiency of total PAHs in the soil increased with increasing consumption of PS. However, the bacterial abundance in soil was negatively affected following oxidation for all of the treatments added with PS, with bacterial abundance in the soil decreased by 0.89~2.88 orders of magnitude compared to the untreated soil. Moreover, the number of total bacteria in the soil decreased as PS consumption increased. Different PS activation methods and PS dosages exhibited different influences on the bacterial community composition. Bacteria capable of degrading PAHs under anoxic conditions were composed predominantly by Proteobacteria and Firmicutes. The total amount of Proteobacteria and Firmicutes also decreased with increasing consumption of PS. The results of this study provide important insight into the design of PAHs contaminated soil remediation projects.

Keywords: activation method, chemical oxidation, indigenous bacteria, polycyclic aromatic hydrocarbon

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Authors: Saba Didarataee, Abbas Ali Khodadadi, Yadollah Mortazavi, Fatemeh Mousavi

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Photocatalytic water splitting is one of the most attractive alternative methods for hydrogen evolution. A variety of nanoparticle engineering techniques were introduced to improve the activity of semiconductor photocatalysts. Among these methods, heterojunction formation is an appealing method due to its ability to effectively preventing electron-hole recombination and improving photocatalytic activity. Reaching an optimal ratio of the two target semiconductors for the formation of heterojunctions is still an open question. Considering environmental issues as well as the cost and availability, ZnS and ZnO are frequently studied as potential choices. In this study, first, the ZnS nanoparticle was synthesized in a hydrothermal process; the formation of ZnS nanorods with a diameter of 14-30 nm was confirmed by field emission scanning electron microscope (FESEM). Then two different methods, partial oxidation and chemical precipitation were employed to construct ZnS/ZnO core-shell heterojunction. X-ray diffraction (XRD), BET, and diffuse reflectance spectroscopy (DRS) analysis were carried out to determine crystallite phase, surface area, and bandgap of photocatalysts. Furthermore, the temperature of oxidation was specified by a temperature programmed oxidation (TPO) and was fixed at 510℃, at which mild oxidation occurred. The bandgap was calculated by the Kubelka-Munk method and decreased by increasing oxide content from 3.53 (pure ZnS) to 3.18 (pure ZnO). The optimal samples were determined by testing the photocatalytic activity of hydrogen evolution in a quartz photoreactor with side irradiation of UVC lamps with a wavelength of 254 nm. In both procedures, it was observed that the photocatalytic activity of the ZnS/ZnO composite was sensibly higher than the pure ZnS and ZnO, which is attributed to forming a type-II heterostructure. The best ratio of oxide to sulfide was 0.24 and 0.37 in partial oxidation and chemical precipitation, respectively. The highest hydrogen evolution was 1081 µmol/gr.h, gained from partial oxidizing of ZnS nanoparticles at 510℃ for 30 minutes.

Keywords: heterostructure, hydrogen, partial oxidation, photocatalyst, water splitting, ZnS

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Authors: Helena M. Wilhelm, Paulo O. Fernandes, Laís P. Dill, Kethlyn G. Moscon

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The use of vegetable oil (or natural ester) as an insulating fluid in electrical transformers is a trend that aims to contribute to environmental preservation since it is biodegradable and non-toxic. Besides, vegetable oil has high flash and combustion points, being considered a fire safety fluid. However, vegetable oil is usually less stable towards oxidation than mineral oil. Both insulating fluids, mineral and vegetable oils, need to be tested periodically according to specific standards. Oxidation stability can be determined by the induction period measured by conductivity method (Rancimat) by monitoring the effectivity of oil’s antioxidant additives, a methodology already developed for food application and biodiesel but still not standardized for insulating fluids. Besides adequate oxidation stability, fluids must be compatible with transformer's construction materials under normal operating conditions to ensure that damage to the oil and parts of the transformer does not occur. ASTM standard and Brazilian normative differ in parameters evaluated, which reveals the need to regulate tests for each oil type. The aim of this study was to assess oxidation stability and compatibility of vegetable oils to suggest the best way to assure a viable performance of vegetable oil as transformer insulating fluid. The determination of the induction period for several vegetable insulating oils from the local market by using Rancimat was carried out according to BS EN 14112 standard, at different temperatures (110, 120, and 130 °C). Also, the compatibility of vegetable oil was assessed according to ASTM and ABNT NBR standards. The main results showed that the best temperature for use in the Rancimat test is 130 °C, which allows a better observation of conductivity change. The compatibility test results presented differences between vegetable and mineral oil standards that should be taken into account in oil testing since materials compatibility and oxidation stability are essential for equipment reliability.

Keywords: compatibility, Rancimat, natural ester, vegetable oil

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Authors: Tatyana T. Tabakova, Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Krasimir I. Ivanov, Yordanka G. Karakirova, Petya Cv. Petrova, Georgi V. Avdeev

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The catalytic oxidation of CO and volatile organic compounds (VOCs) is considered as one of the most efficient ways to reduce harmful emissions from various chemical industries. The effectiveness of gold-based catalysts for many reactions of environmental significance was proven during the past three decades. The aim of this work was to combine the favorable features of Au and Cu-Ce mixed oxides in the design of new catalytic materials of improved efficiency and economic viability for removal of air pollutants in waste gases from formaldehyde production. Supported oxides of copper and cerium with Cu: Ce molar ratio 2:1 and 1:5 were prepared by wet impregnation of g-alumina. Gold (2 wt.%) catalysts were synthesized by a deposition-precipitation method. Catalysts characterization was carried out by texture measurements, powder X-ray diffraction, temperature programmed reduction and electron paramagnetic resonance spectroscopy. The catalytic activity in the oxidation of CO, CH₃OH and (CH₃)₂O was measured using continuous flow equipment with fixed bed reactor. Both Cu-Ce/alumina samples demonstrated similar catalytic behavior. The addition of gold caused significant enhancement of CO and methanol oxidation activity (100 % degree of CO and CH₃OH conversion at about 60 and 140 ^oC, respectively). The composition of Cu-Ce mixed oxides affected the performance of gold-based samples considerably. Gold catalyst on Cu-Ce/γ-Al₂O₃ 1:5 exhibited higher activity for CO and CH₃OH oxidation in comparison with Au on Cu-Ce/γ-Al₂O₃ 2:1. The better performance of Au/Cu-Ce 1:5 was related to the availability of highly dispersed gold particles and copper oxide clusters in close contact with ceria.

Keywords: CO and VOCs oxidation, copper oxide, Ceria, gold catalysts

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Authors: Agarana Michael C., Akinlabi Esther T., Pule Kholopane

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Innovation in manufacturing process technologies and associated product design affects the prospects for manufacturing today and in near future. In this study some theoretical methods, useful as tools in advanced manufacturing, are considered. In particular, some basic Mathematical, Operational Research, Heuristic, and Statistical techniques are discussed. These techniques/methods are very handy in many areas of advanced manufacturing processes, including process planning optimization, modelling and analysis. Generally the production rate requires the application of Mathematical methods. The Emerging Trends Processes in Advanced Manufacturing can be enhanced by using Mathematical Modelling and Optimization techniques.

Keywords: mathematical modelling, optimization, emerging trends, advanced manufacturing

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Authors: Cahit Demetgul, Sahin Bayraktar, Neslihan Beyazit

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Metalloenzymes are enzyme proteins containing metal ions, which are directly bound to the protein or to enzyme-bound nonprotein components. One of the major metalloenzymes that play a key role in oxidation reactions is catechol oxidase, which shows catecholase activity i.e. oxidation of a broad range of catechols to quinones through the four-electron reduction of molecular oxygen to water. Studies on the model compounds mimicking the catecholase activity are very useful and promising for the development of new, more efficient bioinspired catalysts, for in vitro oxidation reactions. In this study, a new tetradentate asymmetrical Schiff-base and its Cu(II) complex were synthesized by condensation of 4-nitro-1,2-phenylenediamine with 6-formyl-7-hydroxy-5-methoxy-2-methylbenzopyran-4-one and by using an appropriate Cu(II) salt, respectively. The prepared compounds were characterized by elemental analysis, FT-IR, NMR, UV-Vis and magnetic susceptibility. The catecholase-mimicking activity of the new Schiff Base Cu(II) complex was performed for the oxidation of 3,5-di-tert-butylcatechol (3,5-DTBC) in methanol at 25 °C, where the electronic spectra were recorded at different time intervals. The yield of the quinone (3,5-DTBQ) was determined from the measured absorbance at 400 nm of the resulting solution. The compatibility of catalytic reaction with Michaelis-Menten kinetics was also investigated. In conclusion, we have found that our new Schiff Base Cu(II) complex presents a significant capacity to catalyze the oxidation reaction of the catechol to o-quinone.

Keywords: catecholase activity, Michaelis-Menten kinetics, Schiff base, transition metals

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Authors: Mairaj Ahmad, L. Paglia, F. Marra, V. Genova, G. Pulci

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This study employed Rene N4 and FSX 414 superalloys, which are used in numerous turbine engine components due of their high strength, outstanding fatigue, creep, thermal, and corrosion-resistant properties. An in-depth examination of corrosion mechanisms with vapor present at high temperature is necessary given the industrial trend toward introducing increasing amounts of hydrogen into combustion chambers in order to boost power generation and minimize pollution in contrast to conventional fuels. These superalloys were oxidized in recent tests for 500, 1000, 2000, 3000 and 4000 hours at 982±5°C temperatures with a steady airflow at a flow rate of 10L/min and 1.5 bar pressure. These superalloys were also examined for wet corrosion for 500, 1000, 2000, 3000, and 4000 hours in a combination of air and water vapor flowing at a 10L/min rate. Weight gain, X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray spectroscopy (EDS) were used to assess the oxidation and heat corrosion resistance capabilities of these alloys before and after 500, 1000, and 2000 hours. The oxidation/corrosion processes that accompany the formation of these oxide scales are shown in the graph of mass gain vs time. In both dry and wet oxidation, oxides like Al2O3, TiO2, NiCo2O4, Ni3Al, Ni3Ti, Cr2O3, MnCr2O4, CoCr2O4, and certain volatile compounds notably CrO2(OH)2, Cr(OH)3, Fe(OH)2, and Si(OH)4 are formed.

Keywords: hot corrosion, oxidation, turbine materials, high temperature corrosion, super alloys

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Authors: Desplanches Maxime

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Accurate estimation of the remaining useful life of lithium-ion batteries for electronic devices is crucial. Data-driven methodologies encounter challenges related to data volume and acquisition protocols, particularly in capturing a comprehensive range of aging indicators. To address these limitations, we propose a hybrid approach that integrates an electrochemical model with state-of-the-art data analysis techniques, yielding a comprehensive database. Our methodology involves infusing an aging phenomenon into a Newman model, leading to the creation of an extensive database capturing various aging states based on non-destructive parameters. This database serves as a robust foundation for subsequent analysis. Leveraging advanced data analysis techniques, notably principal component analysis and t-Distributed Stochastic Neighbor Embedding, we extract pivotal information from the data. This information is harnessed to construct a regression function using either random forest or support vector machine algorithms. The resulting predictor demonstrates a 5% error margin in estimating remaining battery life, providing actionable insights for optimizing usage. Furthermore, the database was built from the Newman model calibrated for aging and performance using data from a European project called Teesmat. The model was then initialized numerous times with different aging values, for instance, with varying thicknesses of SEI (Solid Electrolyte Interphase). This comprehensive approach ensures a thorough exploration of battery aging dynamics, enhancing the accuracy and reliability of our predictive model. Of particular importance is our reliance on the database generated through the integration of the electrochemical model. This database serves as a crucial asset in advancing our understanding of aging states. Beyond its capability for precise remaining life predictions, this database-driven approach offers valuable insights for optimizing battery usage and adapting the predictor to various scenarios. This underscores the practical significance of our method in facilitating better decision-making regarding lithium-ion battery management.

Keywords: Li-ion battery, aging, diagnostics, data analysis, prediction, machine learning, electrochemical model, regression

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Authors: Loai Ben Naji, Osama M. Ibrahim, Khaled J. Al-Fadhalah

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The objective of this paper is to investigate the formation and adhesion of a protective aluminum-oxide (Al₂O₃, alumina) layer on the surface of Iron-Chromium-Aluminum Alloy (Fe-Cr-Al) sintered-metal-fibers. The oxide-scale layer was developed via multi-stage thermal oxidation at 930 ^oC for 1 hour, followed by 1 hour at 960 ^oC, and finally at 990 ^oC for 2 hours. Scanning Electron Microscope (SEM) images show that the multi-stage thermal oxidation resulted in the formation of predominantly Al₂O₃ platelets-like and whiskers. SEM images also reveal non-uniform oxide-scale growth on the surface of the fibers. Furthermore, peeling/spalling of the alumina protective layer occurred after minimum handling, which indicates weak adhesion forces between the protective layer and the base metal alloy.  Energy Dispersive Spectroscopy (EDS) analysis of the heat-treated Fe-Cr-Al sintered-metal-fibers confirmed the high aluminum content on the surface of the protective layer, and the low aluminum content on the exposed base metal alloy surface. In conclusion, the failure of the oxide-scale protective layer exposes the base metal alloy to further oxidation, and the fragile non-uniform oxide-scale is not suitable as a support for catalysts.

Keywords: high-temperature oxidation, iron-chromium-aluminum alloy, alumina protective layer, sintered-metal-fibers

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: Ahmed Ait Hou

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The wing leading edge and nose cone of the space shuttle are fabricated from a reinforced carbon/carbon material. This material attains its durability from a diffusion coating of silicon carbide (SiC) and a glass sealant. During re-entry into the atmosphere, this material is subject to an oxidizing high-temperature environment. The use of thermochemical calculations resulting at the HSC CHEMISTRY software and its database allows us to interpret the phenomena of oxidation and chloridation observed on the wing leading edge and nose cone of the space shuttle during its mission in space. First study is the monitoring of the oxidation reaction of SiC. It has been demonstrated that thermal oxidation of the SiC gives the two compounds SiO₂(s) and CO(g). In the extreme conditions of very low oxygen partial pressures and high temperatures, there is a reaction between SiC and SiO₂, leading to SiO(g) and CO(g). We had represented the phase stability diagram of Si-C-O system calculated by the use of the HSC Chemistry at 1300°C. The principal characteristic of this diagram of predominance is the line of SiC + SiO₂ coexistence. Second study is the monitoring of the chloridation reaction of SiC. The other problem encountered in addition to oxidation is the phenomenon of chloridation due to the presence of NaCl. Indeed, after many missions, the leading edge wing surfaces have exhibited small pinholes. We have used the HSC Chemistry database to analyze these various reactions. Our calculations concorde with the phenomena we announced in research work resulting in NASA LEWIS Research center.

Keywords: thermochchemicals calculations, HSC software, oxidation and chloridation, wings in space

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Authors: Bhairi Lakshminarayana, Surajit Sarker, Ch. Subrahmanyam

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The present study reports the development of noble metal free nano catalysts for low-temperature CO oxidation and water gas shift reaction. Mn-substituted CeO2 solid solution catalysts were synthesized by co-precipitation, combustion and hydrothermal methods. The formation of solid solution was confirmed by XRD with Rietveld refinement and the percentage of carbon and nitrogen doping was ensured by CHNS analyzer. Raman spectroscopic confirmed the oxygen vacancies. The surface area, pore volume and pore size distribution confirmed by N2 physisorption analysis, whereas, UV-visible diffuse reflectance spectroscopy and XPS data confirmed the oxidation state of the Mn ion. The particle size and morphology (spherical shape) of the material was confirmed using FESEM and HRTEM analysis. Ce0.8Mn0.2O2-δ was calcined at 400 °C, 600 °C and 800 °C. Raman spectroscopy confirmed that the catalyst calcined at 400 °C has the best redox properties. The activity of the designed catalysts for CO oxidation (0.2 vol%), carried out with GHSV of 21,000 h-1 and it has been observed that co-precipitation favored the best active catalyst towards CO oxidation and water gas shift reaction, due to the high surface area, improved reducibility, oxygen mobility and highest quantity of surface oxygen species. The activation energy of low temperature CO oxidation on Ce0.8Mn0.2O2- δ (combustion) was 5.5 kcal.K-1.mole-1. The designed catalysts were tested for water gas shift reaction. The present study demonstrates that Mn ion substituted ceria at 400 °C calcination temperature prepared by co-precipitation method promise to revive a green sustainable energy production approach.

Keywords: Ce0.8Mn0.2O2-ð, CO oxidation, physicochemical characterization, water gas shift reaction (WGS)

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Authors: Abhishek Kumar, Mohamed Awadein, Georg Gramse, Luyang Song, He Sun, Wolfgang Schofberger, Stefan Müllegger

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Electron transfer is a crucial part of chemical reactions which drive everyday processes. With the help of an electro-chemical radio frequency scanning tunneling microscopy (EC-RF-STM) setup, we are observing single electron mediated oxidation-reduction processes in molecules like ferrocene and transition metal corroles. Combining the techniques of scanning microwave microscopy and cyclic voltammetry allows us to monitor such processes with attoampere sensitivity. A systematic study of such phenomena would be critical to understanding the nano-scale behavior of catalysts, molecular sensors, and batteries relevant to the development of novel material and energy applications.

Keywords: radiofrequency, STM, cyclic voltammetry, ferrocene

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Authors: Ivan P. Pozdnyakov, Alexey A. Melnikov, Nikolai V. Tkachenko

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Photochemical reactions with participation of iron (III) carboxylates are important for environmental photochemistry and have a great potential of application in water purification (Advanced Oxidation Processes, photo-Fenton and Fenton-like processes). In spite of this information about excited states and primary intermediates in photochemistry of Fe(III) complexes with carboxylic acids is scarce. This talk presents and discusses the results of several recent authors' publications in a field of ultra fast spectroscopy of natural Fe(III) carboxylates.

Keywords: carboxylates, iron complexes, photochemistry, radical complexes, ultrafast processes

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Authors: Stefan Andersson, Balram Panjwani, Bernd Wittgens, Jan Erik Olsen

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Polycyclic Aromatic hydrocarbons are organic compounds consisting of only hydrogen and carbon aromatic rings. PAH are neutral, non-polar molecules that are produced due to incomplete combustion of organic matter. These compounds are carcinogenic and interact with biological nucleophiles to inhibit the normal metabolic functions of the cells. Norways, the most important sources of PAH pollution is considered to be aluminum plants, the metallurgical industry, offshore oil activity, transport, and wood burning. Stricter governmental regulations regarding emissions to the outer and internal environment combined with increased awareness of the potential health effects have motivated Norwegian metal industries to increase their efforts to reduce emissions considerably. One of the objective of the ongoing industry and Norwegian research council supported "SCORE" project is to reduce potential PAH emissions from an off gas stream of a ferroalloy furnace through controlled combustion. In a dedicated combustion chamber. The sizing and configuration of the combustion chamber depends on the combined properties of the bulk gas stream and the properties of the PAH itself. In order to achieve efficient and complete combustion the residence time and minimum temperature need to be optimized. For this design approach reliable kinetic data of the individual PAH-species and/or groups thereof are necessary. However, kinetic data on the combustion of PAH are difficult to obtain and there is only a limited number of studies. The paper presents an evaluation of the kinetic data for some of the PAH obtained from literature. In the present study, the oxidation is modelled for pure PAH and also for PAH mixed with process gas. Using a perfectly stirred reactor modelling approach the oxidation is modelled including advanced reaction kinetics to study influence of residence time and temperature on the conversion of PAH to CO2 and water. A Chemical Reactor Network (CRN) approach is developed to understand the oxidation of PAH inside the combustion chamber. Chemical reactor network modeling has been found to be a valuable tool in the evaluation of oxidation behavior of PAH under various conditions.

Keywords: PAH, PSR, energy recovery, ferro alloy furnace

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Authors: Hanjie Xie, Raphael Semiat, Ziyi Zhong

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It is well known that many oxidation reactions in nature are closely related to the origin and life activities. One of the features of these natural reactions is that they can proceed under mild conditions employing the oxidant of molecular oxygen (O₂) in the air and enzymes as catalysts. Catalysis is also a necessary part of life for human beings, as many chemical and pharmaceutical industrial processes need to use catalysts. However, most heterogeneous catalytic reactions must be run at high operational reaction temperatures and pressures. It is not strange that, in recent years, research interest has been redirected to green catalysis, e.g., trying to run catalytic reactions under relatively mild conditions as much as possible, which needs to employ green solvents, green oxidants such O₂, particularly air, and novel catalysts. This work reports the efficient binary Fe-Mn metal oxide catalysts for low-temperature formaldehyde (HCHO) oxidation, a toxic pollutant in the air, particularly in indoor environments. We prepared a series of nanosized FeMn oxide catalysts and found that when the molar ratio of Fe/Mn = 1:1, the catalyst exhibited the highest catalytic activity. At room temperature, we realized the complete oxidation of HCHO on this catalyst for 20 h with a high GHSV of 150 L g⁻¹ h⁻¹. After a systematic investigation of the catalyst structure and the reaction, we identified the reaction intermediates, including dioxymethylene, formate, carbonate, etc. It is found that the oxygen vacancies and the derived active oxygen species contributed to this high-low-temperature catalytic activity. These findings deepen the understanding of the catalysis of these binary Fe-Mn metal oxide catalysts.

Keywords: oxygen vacancy, catalytic oxidation, binary transition oxide, formaldehyde

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Authors: Jin Lin, Shouxiang Lu, Kim Meow Liew

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The requirement for the long-term mission of the submarine and spacecraft has made the removal of CO₂ and trace CO the critical technology to ensure the health and life of the crews. In this work, CuMnCe, a metal oxide catalyst, supporting K₂CO₃ sorbent was prepared by the wet-solid state impregnation method to realize the integrated CO and CO₂ removal, which might also reduce the volume/mass load of the purification units in the limited space. The as-prepared samples with different addition amount of K₂CO₃ were tested using the fixed bed reactor to reveal the CO oxidation and CO₂ absorption behavior. And the regeneration and stability experiments were also conducted. The results showed that the samples realized the catalyst and sorbent integration to capture CO and CO₂ at the same time. The addition amount of the sorbent had a weak influence on the CO oxidation performance. While the addition amount affected the CO₂ sorption efficiency and capacity significantly. Meanwhile, the presence of water vapor could reduce the CO oxidation activity of the samples similarly, whether with K2CO3 sorbent addition or not. Furtherly, regeneration and stability experiment results showed that the samples after 3-5 times regeneration exhibited almost the same performance of CO and CO₂ removal. Summarily, CuMnCe catalyst supporting K₂CO₃ sorbent could be a good attempt to control CO and CO₂ pollutants generated from the daily equipment running and staff breathing in the confined space such as submarine and spacecraft.

Keywords: CO oxidation, CO₂ absorptio, potassium carbonate, CuMnCe metal oxide, confined space

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Authors: Ahmed A. Abdel-Khalek, Reham A. Mohamed

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The kinetics of oxidation of the cobalt (II) complexes, [CoII(ADA)(Gly)(H2O)2]-, (ADA = N-(2-acetamido) iminodi-acetic acid and (Gly = Glycine) by periodate in aqueous acetate medium to cobalt (III) have been studied spectrophotometrically at 530 nm over the 30–50°C and a variety pH 4.57-5.25 range and I = 0.50 mol dm-3 under pseudo first order condition by taking large excess of oxidant [IO4-] and it obeys the following rate law: Rate=[CoII(ADA)(Gly)(H2O)2]-[H5IO6]{k4K6+(k5K7K5/[H+])}. Also, the kinetics of oxidation of the cobalt(II) complexes, [CoII(ADA)(Val)(H2O)2]- (ADA = N-(2-acetamido) iminodi-acetic acid and (Val = valine) by periodate in aqueous medium to cobalt (III) have been studied spectrophotometrically at 580 nm over the 30–50°C and a variety pH 4.3-5.12 range and I = 0.50 mol dm-3 under pseudo first order condition by taking large excess of oxidant [IO4-] and it obeys the following rate law: Rate=[CoII(ADA)(Val)(H2O)2]-[H5IO6]{k4K6+(k5K7K5/[H+])}

Keywords: periodate, oxidation, cobalt (II), glycine, valine acid, n-(2-acetamido imino-diacetato)

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Authors: Yousef Naserzadeh, Niloufar Mahmoudi

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Oxidation resistance is one of the important parameters in maintaining the quality of olive oil during its storage. Ensuring the stability of the quality of olive oil is one of the important concerns of the producers and consumers. Prooxidants such as iron and copper accelerate the oxidation reaction, and also anti-oxidants and chelating compounds delay it. In this study, chelating effect of tea extract which contains significant amounts of tannic acid is investigated in comparison with citric acid. To do it, 0.1 ppm copper was added to these four kinds of oil, sunflower, olive, canola, and tallow, and then chelating effect of citric acid (0.01%), tannic acid (0.01%) and tea extract (0.1%) were measured by adding to this composition. To this end, the resistance time of the oils against oxidation was measured at 120 °C and an air flow of 20 liters per hour. And the value of peroxide was measured by oven test in six periods of 24 hours at 105 °C. The results showed that citric acid, tannic acid and tea extract had chelating property and increased the resistance time of the studied oils. As a result, considering chelating property and increasing resistance of oil, tannic acid showed better effect than tea extract and tea extract had better effect than citric acid.

Keywords: tannic acid, chelate, edible oils, black tea extract, TBHQ

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Authors: Marita Pigłowska, Beata Kurc, Maciej Galiński

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The application of carbon materials in the branches of the electrochemical industry shows an increasing tendency each year due to the many interesting properties they possess. These are, among others, a well-developed specific surface, porosity, high sorption capacity, good adsorption properties, low bulk density, electrical conductivity and chemical resistance. All these properties allow for their effective use, among others in supercapacitors, which can store electric charges of the order of 100 F due to carbon electrodes constituting the capacitor plates. Coals (including expanded graphite, carbon black, graphite carbon fibers, activated carbon) are commonly used in electrochemical methods of removing oil derivatives from water after tanker disasters, e.g. phenols and their derivatives by their electrochemical anodic oxidation. Phenol can occupy practically the entire surface of carbon material and leave the water clean of hydrophobic impurities. Regeneration of such electrodes is also not complicated, it is carried out by electrochemical methods consisting in unblocking the pores and reducing resistances, and thus their reactivation for subsequent adsorption processes. Graphite is commonly used as an anode material in lithium-ion cells, while due to the limited capacity it offers (372 mAh g-1), new solutions are sought that meet both capacitive, efficiency and economic criteria. Increasingly, biodegradable materials, green materials, biomass, waste (including agricultural waste) are used in order to reuse them and reduce greenhouse effects and, above all, to meet the biodegradability criterion necessary for the production of lithium-ion cells as chemical power sources. The most common of these materials are cellulose, starch, wheat, rice, and corn waste, e.g. from agricultural, paper and pharmaceutical production. Such products are subjected to appropriate treatments depending on the desired application (including chemical, thermal, electrochemical). Starch is a biodegradable polysaccharide that consists of polymeric units such as amylose and amylopectin that build an ordered (linear) and amorphous (branched) structure of the polymer. Carbon is also used as a catalyst. Elemental carbon has become available in many nano-structured forms representing the hybridization combinations found in the primary carbon allotropes, and the materials can be enriched with a large number of surface functional groups. There are many examples of catalytic applications of coal in the literature, but the development of this field has been hampered by the lack of a conceptual approach combining structure and function and a lack of understanding of material synthesis. In the context of catalytic applications, the integrity of carbon environmental management properties and parameters such as metal conductivity range and bond sequence management should be characterized. Such data, along with surface and textured information, can form the basis for the provision of network support services.

Keywords: carbon materials, catalysis, BET, capacitors, lithium ion cell

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

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

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

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

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

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

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Authors: Moustafa Elhamouly, Masayuki Shimada

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The production of competent oocytes is essential for reproductivity in mammals. Maintenance of mitochondrial efficiency is required to supply the ATP necessary for granulosa cell proliferation during the follicular development process. Treatment with Pyrroloquinoline quinone (PQQ) has been reported to increase the number of ovulated oocytes and pups per delivery in mice by maintaining healthy mitochondrial function. This study aimed to elucidate how PQQ maintains mitochondrial function during ovarian follicle growth. To do this, both in vitro and in vivo experiments were performed with granulosa cells from superovulated immature (3-week-old) mice that were pretreated with or without PQQ. The effects of PQQ on beta-oxidation, mitochondrial function, mitophagy, and mitochondrial biogenesis were examined. PQQ increased beta-oxidation-related genes and CPT1 protein content in granulosa cells and this was associated with a decreased phosphorylation of P38 signaling protein. Using the fatty acid oxidation assay on the flux analyzer, PQQ increased the reliance of beta-oxidation on the endogenous fatty acids and was associated with a mild UCP-dependant mitochondrial uncoupling, ATP production, mitophagy, and mitochondrial biogenesis. PQQ also increased the expression of endogenous antioxidant enzymes. Thus, PQQ induced beta-oxidation in growing granulosa cells relying on endogenous fatty acids. And reduced the Reactive oxygen species (ROS) production by inducing a mild mitochondrial uncoupling with keeping high mitochondrial function. Damaged mitochondria were recycled by the induced mitophagy and replaced by the increased mitochondrial biogenesis. Collectively, PQQ may enhance reproductivity by maintaining the efficiency of mitochondria to produce enough ATP required for normal folliculogenesis.

Keywords: granulosa cells, mitochondrial uncoupling, mitophagy, pyrroloquinoline quinone (PQQ), reactive oxygen species (ROS).

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Authors: Ipek Gunay, Efe B. Orman, Metin Ozer, Bekir Salih, Ali R. Ozkaya

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Phthalocyanines with macrocyclic ring containing at least three heteroatoms have nine or more membered structures. Metal-free phthalocyanines react with metal salts to obtain chelate complexes. This is one of the most important features of metal-free phthalocyanine as ligand structure. Although phthalocyanines have very similar properties with porphyrins, they have some advantages such as lower cost, easy to prepare, and chemical and thermal stability. It’s known that Pc compounds have shown one-electron metal-and/or ligand-based reversible or quasi-reversible reduction and oxidation processes. The redox properties of phthalocyanines are critically related to the desirable properties of these compounds in their technological applications. Thus, Pc complexes have also been receiving increasing interest in the area of fuel cells due to their high electrocatalytic activity in dioxygen reduction and fuel cell applications. In this study, novel phthalocyanine complexes coordinated with Fe(II) and Co (II) to be used as catalyst were synthesized. Aiming this goal, a new nitrile ligand was synthesized starting from 4-hydroxy-3,5-dimethoxy benzyl alcohol and 4-nitrophthalonitrile in the presence of K2CO3 as catalyst. After the isolation of the new type of nitrile and metal complexes, the characterization of mentioned compounds was achieved by IR, H-NMR and UV-vis methods. In addition, the electrochemical behaviour of Pc complexes was identified by cyclic voltammetry, square wave voltammetry and in situ spectroelectrochemical measurements. Furthermore, the catalytic performances of Pc complexes for oxygen reduction were tested by dynamic voltammetry measurements, carried out by the combined system of rotating ring-disk electrode and potentiostat, in a medium similar to fuel-cell working conditions.

Keywords: phthalocyanine, electrocatalysis, electrochemistry, in-situ spectroelectrochemistry

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Authors: Zahrasadat Hosseini, Jie Yuan

Abstract:

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

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

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