Search results for: microwave synthesis

Authors: B. M. Patil

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Calcium Zirconate (CaZrO3) has high protonic conductivities at elevated temperature in water or hydrogen atmosphere. Undoped calcium zirconate acts as a p-type semiconductor in air. In this paper, we reported synthesis of CaZrO3 nanoparticles via modified molecular precursor method. The precursor calcium zirconium oxalate (CZO) was synthesized by exchange reaction between freshly generated aqueous solution of sodium zirconyl oxalate and calcium acetate at room temperature. The controlled pyrolysis of CZO in air at 700°C for one hour resulted in the formation nanocrystalline CaZrO3 powder. CaZrO3 obtained by the present method was characterized by Simultaneous thermogravimetry and differential thermogravimetry (TG-DTA), X-ray diffraction (XRD), infra-red spectroscopy and transmission electron microscopy (TEM). The pellets of synthesized CaZrO3 fabricated, sintered at 1000°C for 5 hr and tested as sensors for NO2 and NH3 gases.

Keywords: CaZrO3, CZO, NO2, NH3

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Authors: Ana Jurkeviciute, Larisa Grigorieva, Ksenia Moskvinа

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Oil shale alkylresorcinols are formed as a by-product in oil shale processing. They are unique raw material for chemical industry. Polycondensation resins obtaining is one of the worthwhile directions of oil shale alkylresorcinols use. These resins are widely applied in many branches of industry such as wood-working, metallurgic, tire, rubber products, construction etc. Possibility of resins obtaining using overall alkylresorcinols will allow to cheapen finished products on their base and to widen the range of resins offered on the market. Synthesis of polycondensation resins on the basis of alkylresorcinols was conducted by several methods in the process of investigations. In the formulations a part of resorcinol was replaced by fractions of oil shale alkylresorcinols containing different amount of 5-methylresorcinol (40-80 mass %). Some resins were modified by aromatic alkene at the stage of synthesis. Thermal stability and degradation behavior of resins were investigated by thermogravimetric analysis (TGA) method both in an inert nitrogen environment and in an oxidative environment of air. TGA integral curves were obtained and processed in dynamic mode for interval of temperatures from 25 to 830 °C. Rate of temperature rise was 5°C/min, gas flow rate - 50 ml/min. Resins power for carbonization was evaluated by carbon residue. Physical-chemical parameters of the resins were determined. Content of resorcinol and 5-methylresorcinol not reacted in the process of synthesis were determined by gas chromatography method.

Keywords: resorcinol, oil shale alkylresorcinols, aromatic alkene, polycondensation resins, modified resins

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Authors: Kyaw Zin Htut

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In this article, the synthesis of the efficiency of intelligent diagnostic system in the aircraft measuring devices is described. The technology developments of the diagnostic system are considered based on the model errors of the gyro instruments, which are used to measure the parameters of the aircraft. The synthesis of the diagnostic intelligent system is considered on the example of the problem of assessment and forecasting errors of the gyroscope devices on the onboard aircraft. The result of the system is to detect of faults of the aircraft measuring devices as well as the analysis of the measuring equipment to improve the efficiency of its work.

Keywords: diagnostic, dynamic system, errors of gyro instruments, model errors, assessment, prognosis

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Authors: Mohamed Arbi Khlifi, Badr M. Alshammari

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This paper discusses the general methods to saturation in the steady-state, two axis (d & q) frame models of synchronous machines. In particular, the important role of the magnetic coupling between the d-q axes (cross-magnetizing phenomenon), is demonstrated. For that purpose, distinct methods of saturation modeling of dumper synchronous machine with cross-saturation are identified, and detailed models synthesis in d-q axes. A number of models are given in the final developed form. The procedure and the novel models are verified by a critical application to prove the validity of the method and the equivalence between all developed models is reported. Advantages of some of the models over the existing ones and their applicability are discussed.

Keywords: cross-magnetizing, models synthesis, synchronous machine, saturated modeling, state-space vectors

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Authors: Sakshi Gupta, Anupam Agrawal, Ekta Singla

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An exoskeleton design for rehabilitation purpose encounters many challenges, including ergonomically acceptable wearing technology, architectural design human-motion compatibility, actuation type, human-robot interaction, etc. In this paper, a passive architecture for upper limb exoskeleton is proposed for assisting in rehabilitation tasks. Kinematic modelling is detailed for task-based kinematic synthesis of the wearable exoskeleton for self-feeding tasks. The exoskeleton architecture possesses expansion and torsional springs which are able to store and redistribute energy over the human arm joints. The elastic characteristics of the springs have been optimized to minimize the mechanical work of the human arm joints. The concept of hybrid combination of a 4-bar parallelogram linkage and a serial linkage were chosen, where the 4-bar parallelogram linkage with expansion spring acts as a rigid structure which is used to provide the rotational degree-of-freedom (DOF) required for lowering and raising of the arm. The single linkage with torsional spring allows for the rotational DOF required for elbow movement. The focus of the paper is kinematic modelling, analysis and task-based synthesis framework for the proposed architecture, keeping in considerations the essential tasks of self-feeding and self-exercising during rehabilitation of partially healthy person. Rehabilitation of primary functional movements (activities of daily life, i.e., ADL) is routine activities that people tend to every day such as cleaning, dressing, feeding. We are focusing on the feeding process to make people independent in respect of the feeding tasks. The tasks are focused to post-surgery patients under rehabilitation with less than 40% weakness. The challenges addressed in work are ensuring to emulate the natural movement of the human arm. Human motion data is extracted through motion-sensors for targeted tasks of feeding and specific exercises. Task-based synthesis procedure framework will be discussed for the proposed architecture. The results include the simulation of the architectural concept for tracking the human-arm movements while displaying the kinematic and static study parameters for standard human weight. D-H parameters are used for kinematic modelling of the hybrid-mechanism, and the model is used while performing task-based optimal synthesis utilizing evolutionary algorithm.

Keywords: passive mechanism, task-based synthesis, emulating human-motion, exoskeleton

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Authors: Lin Cheng, Zijiang Yang

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Program synthesis is the task to automatically generate programs based on user specification. In this paper, we present a framework that synthesizes programs from flow charts that serve as accurate and intuitive specification. In order doing so, we propose a deep neural network called GRCNN that recognizes graph structure from its image. GRCNN is trained end-to-end, which can predict edge and node information of the flow chart simultaneously. Experiments show that the accuracy rate to synthesize a program is 66.4%, and the accuracy rates to recognize edge and node are 94.1% and 67.9%, respectively. On average, it takes about 60 milliseconds to synthesize a program.

Keywords: program synthesis, flow chart, specification, graph recognition, CNN

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Authors: Taha Ahmed Özbey, Sedat Nazlıbilek, Alparslan Çağrı Yapıcı

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Combline cavity filters have gained significant attention in recent years due to their exceptional narrowband characteristics, high unloaded Q, remarkable out-of-band rejection, and versatile post-manufacturing tuning capabilities. These filters play a vital role in various wireless communication systems, radar applications, and other advanced technologies where stringent frequency selectivity and superior performance are required. This paper represents combined cavity filter design and implementation by coupling matrix synthesis. Limited filter length, 50 dB out-of-band rejection, and agile design were aimed. To do so, CAD tools and intuitive methods were used.

Keywords: cavity, band pass filter, cavity combline filter, coupling matrix synthesis

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Authors: Oibar Martinez, Clara Oliver, Jose Miguel Miranda

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The study of dispersion phenomena in electromagnetic waves reflected by conductors at infrared and lower frequencies is a topic which finds a number of applications. We aim to explain in this work what are the most relevant ones and how this phenomenon is modeled from both optics and electromagnetics points of view. We also explain here how the amplitude of an electromagnetic wave reflected by a lossy conductor could depend on both the frequency of the incident wave, as well as on the electrical properties of the conductor, and we illustrate this phenomenon with a practical example. The mathematical analysis made by a specialist in electromagnetics or a microwave engineer is apparently very different from the one made by a specialist in optics. We show here how both approaches lead to the same physical result and what are the key concepts which enable one to understand that despite the differences in the equations the solution to the problem happens to be the same. Our study starts with an analysis made by using the complex refractive index and the reflectance parameter. We show how this reflectance has a dependence with the square root of the frequency when the reflecting material is a good conductor, and the frequency of the wave is low enough. Then we analyze the same problem with a less known approach, which is based on the reflection coefficient of the electric field, a parameter that is most commonly used in electromagnetics and microwave engineering. In summary, this paper presents a mathematical study illustrated with a worked example which unifies the modeling of dispersion effects made by specialists in optics and the one made by specialists in electromagnetics. The main finding of this work is that it is possible to reproduce the dependence of the Fresnel reflectance with frequency from the intrinsic impedance of the reflecting media.

Keywords: dispersion, electromagnetic waves, microwaves, optics

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Authors: S. Wiak, L. Szymanski, Z. Kolacinski, G. Raniszewski, L. Pietrzak, Z. Staniszewska

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The term ‘cancer’ is given to a collection of related diseases that may affect any part of the human body. It is a pathological behaviour of cells with the potential to undergo abnormal breakdown in the processes that control cell proliferation, differentiation, and death of particular cells. Although cancer is commonly considered as modern disease, there are beliefs that drastically growing number of new cases can be linked to the extensively prolonged life expectancy and enhanced techniques for cancer diagnosis. Magnetic hyperthermia therapy is a novel approach to cancer treatment, which may greatly contribute to higher efficiency of the therapy. Employing carbon nanotubes as nanocarriers for magnetic particles, it is possible to decrease toxicity and invasiveness of the treatment by surface functionalisation. Despite appearing in recent years, magnetic particle hyperthermia has already become of the highest interest in the scientific and medical environment. The reason why hyperthermia therapy brings so much hope for future treatment of cancer lays in the effect that it produces in malignant cells. Subjecting them to thermal shock results in activation of numerous degradation processes inside and outside the cell. The heating process initiates mechanisms of DNA destruction, protein denaturation and induction of cell apoptosis, which may lead to tumour shrinkage, and in some cases, it may even cause complete disappearance of cancer. The factors which have the major impact on the final efficiency of the treatment include temperatures generated inside the tissues, time of exposure to the heating process, and the character of an individual cancer cell type. The vast majority of cancer cells is characterised by lower pH, persistent hypoxia and lack of nutrients, which can be associated to abnormal microvasculature. Since in healthy tissues we cannot observe presence of these conditions, they should not be seriously affected by elevation of the temperature. The aim of this work is to investigate the influence of iron content in iron filled Carbon Nanotubes on the desired nanoparticles for cancer therapy. In the article, the development and demonstration of the method and the model device for hyperthermic selective destruction of cancer cells are presented. This method was based on the synthesis and functionalization of carbon nanotubes serving as ferromagnetic material nanocontainers. The methodology of the production carbon- ferromagnetic nanocontainers (FNCs) includes the synthesis of carbon nanotubes, chemical, and physical characterization, increasing the content of a ferromagnetic material and biochemical functionalization involving the attachment of the key addresses. The ferromagnetic nanocontainers were synthesised in CVD and microwave plasma system. The research work has been financed from the budget of science as a research project No. PBS2/A5/31/2013.

Keywords: hyperthermia, carbon nanotubes, cancer colon cells, radio frequency field

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Authors: Carolin Anna Joy, Rohith K. R, Rehin Sulay, Parvathy Santhoshkumar, G.Anil Kumar, Vibin Ipe Thomas

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Ullmann coupling reactions are gaining great relevance owing to their contribution in the synthesis of biologically and pharmaceutically important compounds. Palladium and many other heavy metals have proven their excellent ability in coupling reaction, but the toxicity matters. The first-row transition metal also possess toxicity, except in the case of iron and manganese. The suitability of manganese as a catalyst is achieving great interest in oxidation, reduction, C-H activation, coupling reaction etc. In this presentation, we discuss the thermo chemistry of ligand free manganese catalyzed C-O coupling reaction between phenol and aryl halide for the synthesis of biaryl ethers using Density functional theory techniques. The mechanism involves an oxidative addition-reductive elimination step. The transition state for both the step had been studied and confirmed using Intrinsic Reaction Coordinate (IRC) calculation. The barrier height for the reaction had also been calculated from the rate determining step. The possibility of other mechanistic way had also been studied. To achieve further insight into the mechanism, substrate having various functional groups is considered in our study to direct their effect on the feasibility of the reaction.

Keywords: Density functional theory, Molecular Modeling, ligand free, biaryl ethers, Ullmann coupling

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Authors: Parvesh Singh, Vipan Kumar, Vishu Mehra

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Quinoline-4-ones represent an important class of heterocyclic scaffolds that have attracted significant interest due to their various biological and pharmacological activities. This heterocyclic unit also constitutes an integral component in drugs used for the treatment of neurodegenerative diseases, sleep disorders and in antibiotics viz. norfloxacin and ciprofloxacin. The synthetic accessibility and possibility of fictionalization at varied positions in quinoline-4-ones exemplifies an elegant platform for the designing of combinatorial libraries of functionally enriched scaffolds with a range of pharmacological profles. They are also considered to be attractive precursors for the synthesis of medicinally imperative molecules such as non-steroidal androgen receptor antagonists, antimalarial drug Chloroquine and martinellines with antibacterial activity. 2-Aryl-2,3-dihydroquinolin-4(1H)-ones are present in many natural and non-natural compounds and are considered to be the aza-analogs of favanones. The β-lactam class of antibiotics is generally recognized to be a cornerstone of human health care due to the unparalleled clinical efficacy and safety of this type of antibacterial compound. In addition to their biological relevance as potential antibiotics, β-lactams have also acquired a prominent place in organic chemistry as synthons and provide highly efficient routes to a variety of non-protein amino acids, such as oligopeptides, peptidomimetics, nitrogen-heterocycles, as well as biologically active natural and unnatural products of medicinal interest such as indolizidine alkaloids, paclitaxel, docetaxel, taxoids, cyptophycins, lankacidins, etc. A straight forward route toward the synthesis of quinoline-4-ones via the triflic acid assisted Fries rearrangement of N-aryl-βlactams has been reported by Tepe and co-workers. The ring expansion observed in this case was solely attributed to the inherent ring strain in β-lactam ring because -lactam failed to undergo rearrangement under reaction conditions. Theabovementioned protocol has been recently extended by our group for the synthesis of benzo[b]-azocinon-6-ones via a tandem Michael addition–Fries rearrangement of sorbyl anilides as well as for the single-pot synthesis of 2-aryl-quinolin-4(3H)-ones through the Fries rearrangement of 3-dienyl-βlactams. In continuation with our synthetic endeavours with the β-lactam ring and in view of the lack of convenient approaches for the synthesis of C-3 functionalized quinolin-4(1H)-ones, the present work describes the single-pot synthesis of C-3 functionalized quinolin-4(1H)-ones via the trific acid promoted Fries rearrangement of C-3 vinyl/isopropenyl substituted β-lactams. In addition, DFT calculations and MD simulations were performed to investigate the stability profles of synthetic compounds.

Keywords: dihydroquinoline, fries rearrangement, azetidin-2-ones, quinoline-4-ones

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Authors: Durata Haciu, Berti Manisa, Ozgur Birer

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ZnO nanoparticles have been synthesized by ultrasonic irradiation from simple linear alcohols and water/ethanolic mixtures, at 50 oC. By changing the composition of the solvent, the shape could be altered. While no product was obtained from methanolic solutions, in ethanol, sheet like lamellar structures prevail.n-propanol and n-butanol resulted in needle like structures. The morphology of ZnO could be thus tailored in a simple way, by varying the solvent, under ultrasonic irradiation, in a relatively less time consuming method. Variation of the morphology and size of Zn also provides a means for modulating the band-gap. Although the chemical effects of ultrasound do not come from direct interaction with molecular species, the high energy derived from acoustic cavitation creates a unique interaction of energy and matter with great potential for synthesis.

Keywords: ultrasound, ZnO, linear alcohols, morphology

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Authors: Yu Zhang, Il Kim

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Polypeptides with defined peptide sequences illustrate the power of remarkable applications in drug delivery, tissue engineering, sensing and catalysis. Especially the cyclic polypeptides, the distinctive topological architecture imparts many characteristic properties comparing to linear polypeptides. Here, a facile and highly efficient strategy for the synthesis of linear and cyclic polypeptides is reported using N-heterocyclic carbenes (NHCs)-mediated ring-opening polymerization (ROP) of α-amino acid N-carboxyanhydrides (NCA) in the presence or absence of primary amine initiator. The polymerization proceeds rapidly in a quasi-living manner, allowing access to linear and cyclic polypeptides of well-defined chain length and narrow polydispersity, as evidenced by nuclear magnetic resonance spectrum (1H NMR and 13C NMR spectra) and size exclusion chromatography (SEC) analysis. The cyclic architecture of the polypeptides was further verified by matrix-assisted laser desorption ionization-time of flight (MALDI-TOF) mass spectra (MALDI-TOF MS) and electrospray ionization (ESI) mass spectra, as well as viscosity studies. This approach can also simplify workup procedures and make bulk scale synthesis possible, which thereby opens avenues for practical uses in diverse areas, opening up the new generation of polypeptide synthesis.

Keywords: α-amino acid N-carboxyanhydrides, living polymerization, polypeptides, N-heterocyclic carbenes, ring-opening polymerization

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Authors: Ali Zazi, Ouiza Cherifi

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Natural gas currently represents a raw material of choice for the manufacture of a wide range of chemical products via synthesis gas, among the routes of transformation of methane into synthesis gas The reaction of the oxidation of methane by gas vapor 'water. This work focuses on the study of the effect of cerieum on the nickel-based catalyst supported by silica for the methane vapor reforming reaction, with a variation of certain parameters of the reaction. The reaction temperature, the H₂O / CH₄ ratio and the flow rate of the reaction mixture (CH₄-H₂O). Two catalysts were prepared by impregnation of Degussa silica with a solution of nickel nitrates and a solution of cerium nitrates [Ni (NO₃) 2 6H₂O and Ce (NO₃) 3 6H₂O] so as to obtain the 1.5% nickel concentrations. For both catalysts and plus 1% cerium for the second catalyst. These Catalysts have been characterized by physical and chemical analysis techniques: BET technique, Atomic Absorption, IR Spectroscopy, X-ray diffraction. These characterizations indicated that the nitrates had impregnated the silica. And that the NiO and Ce₂O3 phases are present and Ni°(after reaction). The BET surface of the silica decreases without being affected. The catalytic tests carried out on the two catalysts for the steam reforming reactions show that the addition of cerium to the nickel improves the catalytic performances of the nickel. And that these performances also depend on the parameters of the reaction, namely the temperature, the rate of the reaction mixture, and the ratio (H₂O / CH₄).

Keywords: heterogeneous catalysis, steam reforming, Methane, Nickel, Cerium, synthesis gas, hydrogen

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Authors: M. D. H. Beg, John O. Akindoyo, Suriati Ghazali, Nitthiyah Jeyaratnam

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Over the period of time, several approaches have been undertaken to mitigate the challenges associated with bone regeneration. This includes but not limited to xenografts, allografts, autografts as well as artificial substitutions like bioceramics, synthetic cements and metals. The former three techniques often come along with peculiar limitation and problems such as morbidity, availability, disease transmission, collateral site damage or absolute rejection by the body as the case may be. Synthetic routes remain the only feasible alternative option for treatment of bone defects. Hydroxyapatite (HA) is very compatible and suitable for this application. However, most of the common methods for HA synthesis are either expensive, complicated or environmentally unfriendly. Interestingly, extraction of HA from bio-wastes have been perceived not only to be cost effective, but also environment friendly. In this research, HA was synthesized from bio-waste: namely bovine bones through three different methods which are hydrothermal chemical processes, ultrasound assisted synthesis and ordinary calcination techniques. Structure and property analysis of the HA was carried out through different characterization techniques such as TGA, FTIR, and XRD. All the methods applied were able to produce HA with similar compositional properties to biomaterials found in human calcified tissues. Calcination process was however observed to be more efficient as it eliminated all the organic components from the produced HA. The HA synthesized is unique for its minimal cost and environmental friendliness. It is also perceived to be suitable for tissue and bone engineering applications.

Keywords: hydroxyapatite, bone, calcination, biowaste

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Authors: F. Deng, R. Sanchez, A. Beltran, S. Maestre

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The high nutritional value associated with seafood is related to the presence of essential trace elements. Moreover, seafood is considered an important source of energy, proteins, and long-chain polyunsaturated fatty acids. Generally, seafood is consumed cooked. Consequently, the nutritional value could be degraded. Seafood, such as fish, shellfish, and seaweed, could be considered as one of the main iodine sources. The deficient or excessive consumption of iodine could cause dysfunction and pathologies related to the thyroid gland. The main objective of this work is to evaluated iodine stability in hake (Merluccius) undergone different culinary techniques. The culinary process considered were: boiling, steaming, microwave cooking, baking, cooking en papillote (twisted cover with the shape of a sweet wrapper) and coating with a batter of flour and deep-frying. The determination of iodine was carried by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Regarding sample handling strategies, liquid-liquid extraction has demonstrated to be a powerful pre-concentration and clean-up approach for trace metal analysis by ICP techniques. Extraction with tetramethylammonium hydroxide (TMAH reagent) was used as a sample preparation method in this work. Based on the results, it can be concluded that the stability of iodine was degraded with the cooking processes. The major degradation was observed for the boiling and microwave cooking processes. The content of iodine in hake decreased up to 60% and 52%, respectively. However, if the boiling cooking liquid is preserved, this loss that has been generated during cooking is reduced. Only when the fish was cooked by following the cooking en papillote process the iodine content was preserved.

Keywords: cooking process, ICP-MS, iodine, hake

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Sonia M. Zanetti, Mario Cilense, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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The contamination of the environment has been one of the biggest problems of our time, mostly due to developments of many industries. SnO2 is an n-type semiconductor with band gap about 3.5 eV and has its electrical conductivity dependent of type and amount of modifiers agents added into matrix ceramic during synthesis process, allowing applications as sensing of gaseous pollutants on ambient. The chemical synthesis by polymeric precursor method consists in a complexation reaction between tin ion and citric acid at 90 °C/2 hours and subsequently addition of ethyleneglycol for polymerization at 130 °C/2 hours. It also prepared polymeric resin of zinc, cobalt and niobium ions. Stoichiometric amounts of the solutions were mixed to obtain the systems (Zn, Nb)-SnO2 and (Co, Nb) SnO2 . The metal immobilization reduces its segregation during the calcination resulting in a crystalline oxide with high chemical homogeneity. The resin was pre-calcined at 300 °C/1 hour, milled in Atritor Mill at 500 rpm/1 hour, and then calcined at 600 °C/2 hours. X-Ray Diffraction (XDR) indicated formation of SnO2 -rutile phase (JCPDS card nº 41-1445). The characterization by Scanning Electron Microscope of High Resolution showed spherical ceramic powder nanostructured with 10-20 nm of diameter. 20 mg of SnO2 -based powder was kept in 20 ml of isopropyl alcohol and then taken to an electrophoretic deposition (EPD) system. The EPD method allows control the thickness films through the voltage or current applied in the electrophoretic cell and by the time used for deposition of ceramics particles. This procedure obtains films in a short time with low costs, bringing prospects for a new generation of smaller size devices with easy integration technology. In this research, films were obtained in an alumina substrate with interdigital electrodes after applying 2 kV during 5 and 10 minutes in cells containing alcoholic suspension of (Zn, Nb)-SnO2 and (Co, Nb) SnO2 of powders, forming a sensing layer. The substrate has designed integrated micro hotplates that provide an instantaneous and precise temperature control capability when a voltage is applied. The films were sintered at 900 and 1000 °C in a microwave oven of 770 W, adapted by the research group itself with a temperature controller. This sintering is a fast process with homogeneous heating rate which promotes controlled growth of grain size and also the diffusion of modifiers agents, inducing the creation of intrinsic defects which will change the electrical characteristics of SnO2 -based powders. This study has successfully demonstrated a microfabricated system with an integrated micro-hotplate for detection of CO and NO2 gas at different concentrations and temperature, with self-heating SnO2 - based nanoparticles films, being suitable for both industrial process monitoring and detection of low concentrations in buildings/residences in order to safeguard human health. The results indicate the possibility for development of gas sensors devices with low power consumption for integration in portable electronic equipment with fast analysis. Acknowledgments The authors thanks to the LMA-IQ for providing the FEG-SEM images, and the financial support of this project by the Brazilian research funding agencies CNPq, FAPESP 2014/11314-9 and CEPID/CDMF- FAPESP 2013/07296-2.

Keywords: chemical synthesis, electrophoretic deposition, self-heating, gas sensor

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Authors: Ujjawal Kumar Bhagat, Kamaluddin, Rama Krishna Peddinti

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The Huisgen’s 1,3-dipolar [3+2] cycloaddition of organic azides and alkynes often give the mixtures of both the regioisomers 1,4- and 1,5- disubstituted 1,2,3-triazoles. Later, in presence of metal salts (click chemistry) such as copper(I)-catalyzed azide-alkyne cycloaddition (CuAAC) was used for the synthesis of 1,4-disubstituted 1,2,3-triazoles as a sole products regioselectively. Also, the ‘click reactions’ of Ruthenium-catalyzed azides-alkynes cycloaddition (RuAAC) is used for the synthesis of 1,5-disubstituted 1,2,3-triazoles as a single isomer. The synthesis of 1,4- and 1.5-disubstituted 1,2,3-triazoles has become the gold standard of ‘click chemistry’ due to its reliability, specificity, and biocompatibility. The 1,4- and 1,5-disubstituted 1,2,3-triazoles have emerged as one of the most powerful entities in the varieties of biological properties like antibacterial, antitubercular, antitumor, antifungal and antiprotozoal activities. Some of the 1,4,5-trisubstituted 1,2,3-triazoles exhibit Hsp90 inhibiting properties. The 1,4-disubstituted 1,2,3-triazoles also play a big role in the area of material sciences. The triazole-derived oligomeric, polymeric structures are the potential materials for the preparation of organic optoelectronics, silicon elastomers and unimolecular block copolymers. By the virtue of hydrogen bonding and dipole interactions, the 1,2,3-triazole moiety readily associates with the biological targets. Since, the 4-aryl-1H-1,2,3-triazoles are stable entities, they are chemically robust and very less reactive. In this regard, the addition of 4-aryl-1H-1,2,3-triazoles as nucleophiles to α,β-unsaturated carbonyls and nucleophilic substitution with the epoxides constitutes a powerful and challenging synthetic approach for the generation of disubstituted 1,2,3-triazoles. Herein, we have developed aza-Michael addition of 4-aryl-1H-1,2,3-triazoles to 2-cycloalken-1-ones in the presence of an organic base (DABCO) in acetonotrile solvent leading to the formation of disubstituted 1,2,3-triazoles. The reaction provides 1,4-disubstituted triazoles, 3-(4-aryl-1H-1,2,3-triazol-1-yl)cycloalkanones in major amount along with 1,5-disubstituted 1,2,3-triazoles, minor regioisomers with excellent combined chemical yields (upto99%). The nucleophilic behavior of 4-aryl-1H-1,2,3-triazoles was also tested in the ring opening of meso-epoxides in the presence of organic bases (DABCO/Et3N) in acetonotrile solvent furnishing the two regioisomers1,4- and 1,5-disubstituted 1,2,3-triazoles. Thus, the novelty of this methodology is synthesis of diversified disubstituted 1,2,3-triazoles under metal free condition.The results will be presented in detail.

Keywords: aza-Michael addition, cycloalkenones, epoxides, triazoles

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Authors: İsmail Çeli̇k, Gülgün Ayhan-Kılcıgi̇l, Arzu Onay-Beşi̇kçi̇

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In this study, some 2-(2-phenyl/substitutedphenyl)- lH-benzo[d]'imidazol-l-yl)-N'-(alkylthiosemicarbazide were designed and prepared. Firstly, 2-phenyl/ suhstitutedphenyl-lH-Benzo[d]imidazole was prepared via oxidative condensation of o-phenylenediamine, benzaldehyde and sodium metabisulfite. Treatment of the benzimidazole compound with ethyl chloroacetate in KOH/DMSO gave the ester compound ethyl 2-(2-substitutedphenyl)-1H-benzo[d]imidazol-l-yl)acetate. Hydrazine hydrate and the ester in ethanol were refluxed for 4 h to give 2-(2-phenyl/substitutedphenyl)-1H-benzo[d]imidazol-l-yl)acetohydrazide. Thiosemicarbazides were obtained by condensing acyl hydrazide with the alkylisothiocyanate in ethanol. Following the structure elucidation, benzimidazole compounds were tested for their EGFR kinase inhibitory activities by using ADP-GloTM Kinase Assay.

Keywords: benzimidazole, EGFR kinase inhibitor, synthesis, thiosemicarbazide

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Authors: Abdelaziz Ghrib, Samir Hattali, Mouloud Ghrib, Mohamed Lamine Aouissia, David Ruch

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In the present study, the solid solutions with a chemical composition of Zr0.8Y0.2-xLaxO2 (x=0, 0.1, 0.2) were synthesized via two routes, by hydrothermal method using NaOH as precipitating agent at 230°C for 15h and by the sol–gel process using citric acid as complexing agent. Compounds have been characterized by powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Thermo gravimetric Analysis (TGA) and Differential Thermal Analysis (DTA) techniques for appropriate characterization of the distinct thermal events occurring during synthesis. All the compounds crystallize in cubic fluorite structure, as indicated by X-ray diffraction studie. The microstructure of oxides synthesized by sol-gel showed porosity that increased with the lanthanum La3+ contents compared to hydrothermal method which gives a single crystal oxide.

Keywords: oxide, hydrothermal, rare earth, solubility, sol-gel, ternary mixture

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Authors: Wallia Majeed

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Humidity sensors based on doped ZnO-rGO composites have shown promise due to their sensitivity to humidity changes. Here, it report on the hydrothermal synthesis of ZnO-rGO and doped ZnO-rGO nanocomposites, incorporating cobalt and iron dopants at 2% concentration. X-ray diffraction confirmed successful doping, while scanning electron microscopy revealed the composite's layered structure with embedded ZnO rods. To evaluate their performance, humidity sensors were fabricated by depositing aluminum electrodes on silicon substrates coated with the composites. The Fe-doped ZnO-rGO sensor exhibited rapid response (27 s) and recovery times (24 s) across a wide humidity range (11% to 97% RH), surpassing ZnO-rGO and Co-doped ZnO-rGO variants in sensitivity (2.2k at 100 Hz). These findings highlight Fe-doped ZnO-rGO composites as ideal candidates for humidity sensing applications, offering enhanced performance crucial for environmental monitoring and industrial processes.

Keywords: humidity sensors, nanocomposites, hydrothermal synthesis, sensitivity

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Authors: Amgad Rezk, Heba Ahmed, Leslie Yeo

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Ultrasound presents a powerful means for material synthesis. In this talk, we showcase a new field demonstrating the possibility for harnessing sound energy sources at considerably higher frequencies (10 MHz to 1 GHz) compared to conventional ultrasound (kHz and up to ~2 MHz) for crystalising and manipulating a variety of nanoscale materials. At these frequencies, cavitation—which underpins most sonochemical processes—is largely absent, suggesting that altogether fundamentally different mechanisms are at dominant. Examples include the crystallization of highly oriented structures, quasi-2D metal-organic frameworks and nanocomposites. These fascinating examples reveal how the highly nonlinear electromechanical coupling associated with high-frequency surface vibration gives rise to molecular ordering and assembly on the nano and microscale.

Keywords: high-frequency acoustics, microfluidics, crystallisation, composite nanomaterials

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Authors: Tareg M. Elsunaki, Suleiman A. Arafa, Mohamed A. Abd-Alla

Abstract:

New interesting thermal stable polyesters containing 1-methyl-4-piperidone moiety in the main chain have been synthesized. These polyesters were synthesized by interfacial polycondensation technique of 3,5-bis(4-hydroxybenzylidene)-1-methyl-4-piperidone (I) and 3,5-bis(4-hydroxy-3-methoxy benzyli-dene)-1-methyl-4-piperidone (II) with terphthaloyl, isophthaloyl, 4,4'-diphenic, adipoyl and sebacoyl dichlorides. The yield and the values of the reduced viscosity of the produced polyesters were found to be affected by the type of an organic phase. In order to characterize these polymers, the necessary model compounds (A), (B) were prepared from (I), (II) respectively and benzoyl chloride. The structure of monomers (I), (II), model compounds and resulting polyesters were confirmed by IR, elemental analysis and 1HNMR spectroscopy. The various characteristic of the resulting polymers including solubility, thermal properties, viscosity and X-ray analysis were also studied.

Keywords: synthesis, characterization, new polyesters, chemistry

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Authors: Jong-Ho Moon, Dong-Ho Lee, Hyunuk Kim, Young Cheol Park, Jong-Seop Lee, Jae-deok Jeon, Hyung-Keun Lee

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A novel membrane reactor process for DMC synthesis from carbon dioxide has been developing in Korea Institute of Energy Research. The scheme of direct synthesis of DMC from CO₂ and Methanol is 'CO₂ + 2MeOH ↔ DMC + H₂O'. Among them, reactants are CO₂ and MeOH, product is DMC, and byproduct is H₂O (water). According to Le Chatelier’s principle, removing byproduct (water) can shift the reaction equilibrium to the right (DMC production). The main purpose of this process is removing water during the reaction. For efficient in situ water removal (dehydration) and DMC separation, zeolite 4A membranes with very small pore diameter and hydrophilicity were introduced. In this study, pervaporation performances of binary and ternary DMC / methanol / water mixtures were evaluated.

Keywords: dimehtyl carbonate, methanol, water, zeolite membrane, pervaporation

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Authors: Hassina Harkat, Samiha Taybe, Salima Loucif, Valérie Beneteau, Patrick Pale

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Indole and its derivatives have attracted great interest because of their importance in the synthetic organic and medicinal chemistry. They are widely used as anti hypertension, anti tubercular, anticancer activity, antiviral, Alzheimer's disease, antioxidant properties, and free radical induced lipid peroxidation. Many drugs and natural products contain indole moiety, such as the vinca alkaloids, fungal metabolites and marine natural products. Generally applicable synthetic methods for indole moiety involve ring closure to form the pyrrole. Indole derivatives can also be accessed by further functionalization of the indole nucleus. Therefore we report a mild and efficient protocol for the synthesis of analogues of indole catalyzed via zeolithe USY doped with CuI under solvent-free conditions.

Keywords: indole, zeolithe, USY-CuI, heterogeneous catalysis

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Authors: Piya Roychoudhury, Ruma Pal

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Cyanobacteria, commonly known as blue green algae were found to be an effective bioreagent for nanoparticle synthesis. Nowadays silver nanoparticles (AgNPs) are very popular due to their antimicrobial and anti-proliferative activity. To exploit these characters in different biotechnological fields, it is very essential to synthesize more stable, non-toxic nano-silver. For this reason silver-gold alloy (Ag-AuNPs) nanoparticles are of great interest as they are more stable, harder and more effective than single metal nanoparticles. In the present communication we described a simple technique for rapid synthesis of biocompatible AgNP and Ag-AuNP employing cyanobacteria, Leptolyngbya and Lyngbya respectively. For synthesis of AgNP the biomass of Leptolyngbya valderiana (200 mg Fresh weight) was exposed to 9 mM AgNO3 solution (pH 4). For synthesis of Ag-AuNP Lyngbya majuscula (200 mg Fresh weight) was exposed to equimolar solution of hydrogen tetra-auro chlorate and silver nitrate (1mM, pH 4). After 72 hrs of exposure thallus of Leptolyngyba turned brown in color and filaments of Lyngbya turned pink in color that indicated synthesis of nanoparticles. The produced particles were extracted from the cyanobacterial biomass using nano-capping agent, sodium citrate. Firstly, extracted brown and pink suspensions were taken for Energy Dispersive X-ray (EDAX) analysis to confirm the presence of silver in brown suspension and presence of both gold and silver in pink suspension. Extracted nanoparticles showed a distinct single plasmon band (AgNP at 411 nm; Ag-Au NP at 481 nm) in Uv-vis spectroscopy. It was revealed from Transmission electron microscopy (TEM) that all the synthesized particles were spherical in nature with a size range of ~2-25 nm. In X-ray powder diffraction (XRD) analysis four intense peaks appeared at 38.2°, 44.5°, 64.8°and 77.8° which confirmed the crystallographic nature of synthesized particles. Presence of different functional groups viz. N-H, C=C, C–O, C=O on the surface of nanoparticles were recorded by Fourier transform infrared spectroscopy (FTIR). Scanning Electron microscopy (SEM) images showed the surface topography of metal treated filaments of cyanobacteria. The stability of the particles was observed by Zeta potential study. Antibiotic property of synthesized particles was tested by Agar well diffusion method against gram negative bacteria Pseudomonas aeruginosa. Overall, this green-technique requires low energy, less manufacturing cost and produces rapidly eco-friendly metal nanoparticles.

Keywords: cyanobacteria, silver nanoparticles, silver-gold alloy nanoparticles, spectroscopy

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Authors: Hamad Almohamadi, Nabeel H. Alharthi, Abdulrahman Aljabri

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In this study, two-dimensional CuFeOx is deposited on nickel foam for the fabrication of electrocatalyst for oxygen evolution reaction (OER). The in-situ hydrothermal synthesis of CuFeOx in presence of aloe vera extract was found to yield unique nano-rose-like morphology which aided to improve the electrochemical surface area of the electrode. The phytochemical assisted synthesis of CuFeOx using 75% aloe vera extract resulted in improved OER electrocatalytic performance by attaining the overpotential of 310 mV for 50 mA cm−2 and 410 mV for 100 mA cm−2. The electrode also sustained robust stability throughout the 50 h of chronopotentiometry studies under alkaline electrolyte conditions, thus proving to be prospective electrode material for efficient OER in electrochemical water splitting.

Keywords: water splitting, phytochemicals, oxygen evaluation reaction, Tafel's slope, stability

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Authors: Wega Trisunaryanti, Hesty Kusumastuti, Iip Izul Falah, Muhammad Fajar Marsuki, Rahmad Nuryanto

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Synthesis of Ni supported on mesopore silica-alumina (MSA) for hydrocracking of pyrolyzed α-cellulose had been carried out. The silica and alumina were extracted from Sidoarjo mud. Gelatin from catfish bone was used as a template for the mesopore design. The MSA was synthesized by using hydrothermal method at 100 °C for 24 h and calcined at 550 °C for 4 h then characterized by using X-Ray Diffraction Spectrometer (XRD) and Nitrogen Gas Sorption Analyzer (GAS). The Ni metal was loaded to the MSA by wet impregnation method. The catalytic activity in the hydrocracking reaction of pyrolyzed α-cellulose was carried out at 450 °C for 2 h. The MSA synthesized in this work is an amorphous material with specific surface area, total pore volume, and average pore diameter of 212.29 m²/g, 1.29 cm³/g, and 20.05 nm, respectively. The Ni/MSA catalyst produced 73.02 wt.% of liquid product in hydrocracking of pyrolyzed α-cellulose.

Keywords: catalyst, gelatin, hydrocracking, mesopore silica-alumina, α-cellulose

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

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

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

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Authors: Ruswanto Ruswanto, Richa Mardianingrum, Tita Nofianti, Nur Rahayuningsih

Abstract:

Tuberculosis (TB) is a chronic disease as a result of Mycobacterium tuberculosis. It can affect all age groups, and hence, is a global health problem that causes the death of millions of people every year. One of the drugs used in tuberculosis treatment is isonicotinohydrazide. In this study, N'-benzoylisonicotinohydrazide derivative compounds (a-l) were prepared using acylation reactions between isonicotinohydrazide and benzoyl chloride derivatives, through the reflux method. Molecular docking studies suggested that all of the compounds had better interaction with Mycobacterium tuberculosis enoyl-acyl carrier protein reductase (InhA) than isonicotinohydrazide. It can be concluded that N'-benzoylisonicotinohydrazide derivatives (a-l) could be used as anti-tuberculosis candidates. From the docking results revealed that all of the compounds interact well with InhA, with compound g (N'-(3-nitrobenzoyl)isonicotinohydrazide) exhibiting the best interaction.

Keywords: anti-tuberculosis , docking, InhA, N'-benzoylisonicotinohydrazide, synthesis

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