Search results for: raman spectra

Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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The structural characterization of silicon nano crystals (SiNCs) have been carried out using transmission electron microscope (TEM) and atomic force microscopy (AFM). SiNCs are crystalline with an average diameter of 65 nm. Erbium trichloride was added to silicon nano crystals using a simple chemical procedure. Erbium is useful in this context because it has a narrow emission band at ⋍1536 nm which corresponds to a standard optical telecommunication wavelength. The optical properties of SiNCs and erbium-mixed SiNCs samples have been characterized using UV-vis spectroscopy, confocal Raman spectroscopy and photoluminescence spectroscopy (PL). SiNCs and erbium-mixed SiNCs samples exhibit an orange PL emission peak at around 595 nm that arise from radiative recombination of Si. Erbium-mixed SiNCs also shows a weak PL emission peak at ⋍1536 nm that attributed to the intra-4f transition in erbium ions. The intensity of the PL peak of Si in erbium-mixed SiNCs is increased in the intensity up to ×3 as compared to pure SiNCs. It was observed that intensity of 1536 nm peak decreased dramatically in the presence of silicon nano crystals and the PL emission peak of silicon nano crystals is increased. Therefore, the resulted data present that the energy transfer from erbium ions to SiNCs due to the chemical mixing method which used in this work.

Keywords: Silicon Nanocrystals (SiNCs), Erbium Ion, photoluminescence, energy transfer

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

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The aim of this study was to use voltammetry as a method to understand the behaviour of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP, which was only applied on two of the three coupons at the protection potential -0.8 V vs Cu/CuSO₄ for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP, while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from the ohmic drop. Voltammetry was finally performed on the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduced the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect from the decreased potential and an induced effect associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy

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Authors: M. A. Karakassides, M. Baikousi, A. Kouloumpis, D. Gournis

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Nanocomposites of Carbon Nanorods (CNRs) with Polystyrene (PS), have been synthesized successfully by means of in situ polymerization process and characterized. Firstly, carbon nanorods with graphitic structure were prepared by the standard synthetic procedure of CMK-3 using MCM-41 as template, instead of SBA-15, and sucrose as carbon source. In order to create an organophilic surface on CNRs, two parts of modification were realized: surface chemical oxidation (CNRs-ox) according to the Staudenmaier’s method and the attachment of octadecylamine molecules on the functional groups of CNRs-ox (CNRs-ODA The nanocomposite materials of polystyrene with CNRs-ODA, were prepared by a solution-precipitation method at three nanoadditive to polymer loadings (1, 3 and 5 wt. %). The as derived nanocomposites were studied with a combination of characterization and analytical techniques. Especially, Fourier-transform infrared (FT-IR) and Raman spectroscopies were used for the chemical and structural characterization of the pristine materials and the derived nanocomposites while the morphology of nanocomposites and the dispersion of the carbon nanorods were analyzed by atomic force and scanning electron microscopy techniques. Tensile testing and thermogravimetric analysis (TGA) along with differential scanning calorimetry (DSC) were also used to examine the mechanical properties and thermal stability -glass transition temperature of PS after the incorporation of CNRs-ODA nanorods. The results showed that the thermal and mechanical properties of the PS/ CNRs-ODA nanocomposites gradually improved with increasing of CNRs-ODA loading.

Keywords: nanocomposites, polystyrene, carbon, nanorods

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Authors: Leslie Raphael de M. Ferraz, Salvana Priscylla M. Costa, Tarcyla de A. Gomes, Giovanna Christinne R. M. Schver, Cristóvão R. da Silva, Magaly Andreza M. de Lyra, Danilo Augusto F. Fontes, Larissa A. Rolim, Amanda Carla Q. M. Vieira, Miracy M. de Albuquerque, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a drug used as first-line treatment of AIDS. However, it has poor aqueous solubility and wettability, presenting problems in the gastrointestinal tract absorption and bioavailability. One of the most promising strategies to improve the solubility is the use of solid dispersions (SD). Therefore, this study aimed to characterize SD EFZ with the polymers: PVP-K30, PVPVA 64 and SOLUPLUS in order to find an optimal formulation to compose a future pharmaceutical product for AIDS therapy. Initially, Physical Mixtures (PM) and SD with the polymers were obtained containing 10, 20, 50 and 80% of drug (w/w) by the solvent method. The best formulation obtained between the SD was selected by in vitro dissolution test. Finally, the drug-carrier system chosen, in all ratios obtained, were analyzed by the following techniques: Differential Scanning Calorimetry (DSC), polarization microscopy, Scanning Electron Microscopy (SEM) and spectrophotometry of absorption in the region of infrared (IR). From the dissolution profiles of EFV, PM and SD, the values of area Under The Curve (AUC) were calculated. The data showed that the AUC of all PM is greater than the isolated EFV, this result is derived from the hydrophilic properties of the polymers thus favoring a decrease in surface tension between the drug and the dissolution medium. In adittion, this ensures an increasing of wettability of the drug. In parallel, it was found that SD whom had higher AUC values, were those who have the greatest amount of polymer (with only 10% drug). As the amount of drug increases, it was noticed that these results either decrease or are statistically similar. The AUC values of the SD using the three different polymers, followed this decreasing order: SD PVPVA 64-EFV 10% > SD PVP-K30-EFV 10% > SD Soluplus®-EFV 10%. The DSC curves of SD’s did not show the characteristic endothermic event of drug melt process, suggesting that the EFV was converted to its amorphous state. The analysis of polarized light microscopy showed significant birefringence of the PM’s, but this was not observed in films of SD’s, thus suggesting the conversion of the drug from the crystalline to the amorphous state. In electron micrographs of all PM, independently of the percentage of the drug, the crystal structure of EFV was clearly detectable. Moreover, electron micrographs of the SD with the two polymers in different ratios investigated, we observed the presence of particles with irregular size and morphology, also occurring an extensive change in the appearance of the polymer, not being possible to differentiate the two components. IR spectra of PM corresponds to the overlapping of polymer and EFV bands indicating thereby that there is no interaction between them, unlike the spectra of all SD that showed complete disappearance of the band related to the axial deformation of the NH group of EFV. Therefore, this study was able to obtain a suitable formulation to overcome the solubility limitations of the EFV, since SD PVPVA 64-EFZ 10% was chosen as the best system in delay crystallization of the prototype, reaching higher levels of super saturation.

Keywords: characterization, dissolution, Efavirenz, solid dispersions

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Authors: Ehsan Sadie

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Developments in the field of damping technology and advances in the area of dampers in equipping many structures have been the result of efforts and testing by researchers in this field. In this paper, a sample of a two-story building is simulated with the help of SAP2000 software, and the effect of a viscous damper on the performance of the structure is explained. The effect of dampers on the response of the structure is investigated. This response involves the horizontal displacement of floors. In this case, the structure is modeled once without a damper and again with a damper. In this regard, the results are presented in the form of tables and graphs. Since the seismic behavior of the structure is studied, the responses show the appropriate effect of viscous dampers in reducing the displacement of floors, and also the energy dissipation in the structure with dampers compared to structures without dampers is significant. Therefore, it is economical to use viscous dampers in areas that have a higher relative earthquake risk.

Keywords: bending frame, displacement criterion, dynamic response spectra, earthquake, non-linear history spectrum, SAP2000 software, structural response, viscous damper

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Authors: Debajit Kalita, Macmillan Nongkhlaw, S. R. Joshi

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Mercury (Hg) is a highly toxic heavy metal released both from naturally occurring volcanoes and anthropogenic activities like alkali and mining industries as well as biomedical wastes. Exposure to mercury is known to affect the nervous, gastrointestinal and renal systems. In the present study, a bacterial isolate identified using 16S rRNA marker as Paenibacillus jamilae PKR1 isolated from India’s largest sandstone-type uranium deposits, containing an average of 0.1% U3O8, was found to be resistance to Hg contamination under culture conditions. It showed strong hydrophobicity as revealed by SAT, MATH, PAT, SAA adherence assays. The Fourier Transform Infrared (FTIR) spectra showed the presence of hydroxyl, amino and carboxylic functional groups on the cell surface EPS which are known to contribute in the binding of metals. It is proposed that the characterized isolate tolerating up to 4.0mM of mercury provides scope for its application in bioremediation of mercury from contaminated sites.

Keywords: mercury, Domiasiat, uranium, paenibacillus jamilae, hydrophobicity, FTIR

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Authors: Su-Ning Wang, Yao-Qiang Chen

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The CeO2-ZrO2-La2O3-Al2O3 composite oxides are synthesized using co-precipitation method by two different reactors (i.e. continuous stirred-tank reactor and batch reactor), and the corresponding Rh-only three-way catalysts are obtained by wet-impregnation approach. The textural, structural, morphology and redox properties of the support materials, as well as the catalytic performance of the Rh-only catalyst are investigated systematically. The results reveal that the materials (CZLA-C) synthesized by continuous stirred-tank reactor have a better physic-chemical properties than the counterpart material (CZLA-B) prepared by batch reactor. After aging treatment at 1000 ℃ for 5 h, the BET surface area and pore volume of S1 reach up to 76 m2 g-1 and 0.36 mL/g, respectively, which is higher than that of S2. The XRD and Raman results demonstrate that a high structural stability is obtained by S1 because of the negligible lattice variation and the slight grain growth after aging treatment. The SEM and TEM images display that the morphology of S1 is assembled by many homogeneous primary nanoparticles (about 6.12 nm) that are connected to form mesoporous structure The TPR measurement shows that S1 possesses a higher reduction ability than S2. Compared with the catalyst supported on the CZLA-B, the as-prepared CZLA-C demonstrates an improved three-way catalytic activity both before and after aging treatment.

Keywords: composite oxides, reactor, catalysis, catalytic performance

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Authors: Gaurav Malik, Satyendra Mourya, Jyoti Jaiswal, Ramesh Chandra

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The attractive and multifunctional properties of ZnO make it a promising material for the fabrication of highly sensitive and selective efficient gas sensors at room temperature. This presented article focuses on the development of highly selective and sensitive H₂ gas sensor based on the Pd-Pt decorated ZnO framework and its sensing mechanisms. The gas sensing performance of sputter made Pd-Pt/ZnO electrode on anodized porous silicon (PSi) substrate toward H₂ gas is studied under low detection limit (2–500 ppm) of H₂ in the air. The chemiresistive sensor demonstrated sublimate selectivity, good sensing response, and fast response/recovery time with excellent stability towards H₂ at low temperature operation under ambient environment. The elaborate selective measurement of Pd-Pt/ZnO/PSi structure was performed towards different oxidizing and reducing gases. This structure exhibited advance and reversible response to H₂ gas, which revealed that the acquired architecture with ZnO framework is a promising candidate for H₂ gas sensor.

Keywords: sputtering, porous silicon, ZnO framework, XPS spectra, gas sensor

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Authors: K. Petcharaporn, S. Kumchoo

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The acidity (citric acid) is one of the chemical contents that can refer to the internal quality and the maturity index of tomato. The titratable acidity (%TA) can be predicted by a non-destructive method prediction by using the transmittance short wavelength (SW-NIR). Spectroscopy in the wavelength range between 665-955 nm. The set of 167 tomato samples divided into groups of 117 tomatoes sample for training set and 50 tomatoes sample for test set were used to establish the calibration model to predict and measure %TA by partial least squares regression (PLSR) technique. The spectra were pretreated with MSC pretreatment and it gave the optimal result for calibration model as (R = 0.92, RMSEC = 0.03%) and this model obtained high accuracy result to use for %TA prediction in test set as (R = 0.81, RMSEP = 0.05%). From the result of prediction in test set shown that the transmittance SW-NIR spectroscopy technique can be used for a non-destructive method for %TA prediction of tomatoes.

Keywords: tomato, quality, prediction, transmittance, titratable acidity, citric acid

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Authors: S. Athiralakshmi, B.E. Bhojaraja, U. Pruthviraj

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In agriculture, remote sensing is applied for monitoring of plant development, evaluating of physiological processes and growth conditions. Especially valuable are the spatio-temporal aspects of the remotely sensed data in detecting crop state differences and stress situations. In this study, hyperion imagery is used for classifying arecanut crops based on their age so that these maps can be used in yield estimation of crops, irrigation purposes, applying fertilizers etc. Traditional hard classifiers assigns the mixed pixels to the dominant classes. The proposed method uses a sub pixel level classifier called linear spectral unmixing available in ENVI software. It provides the relative abundance of surface materials and the context within a pixel that may be a potential solution to effectively identifying the land-cover distribution. Validation is done referring to field spectra collected using spectroradiometer and the ground control points obtained from GPS.

Keywords: FLAASH, Hyperspectral remote sensing, Linear Spectral Unmixing, Spectral Angle Mapper Classifier.

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Authors: Ahmed Hamida Boudinar, Noureddine Benouzza, Azeddine Bendiabdellah, Mohamed El Amine Khodja

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This paper describes a new diagnosis approach for identification of the progressive stator winding inter-turn short-circuit fault in induction motor. This approach is based on a simple monitoring of the combined information related to both magnitude and phase-angle obtained from the fundamental by the three line currents frequency analysis. In addition, to simplify the interpretation and analysis of the data; a new graphical tool based on a triangular representation is suggested. This representation, depending on its size, enables to visualize in a simple and clear manner, the existence of the stator inter-turn short-circuit fault and its discrimination with respect to a healthy stator. Experimental results show well the benefit and effectiveness of the proposed approach.

Keywords: induction motor, magnitude, phase-angle, spectral analysis, stator fault

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Authors: M. R. S. Nasuha, K. Azman, H. Azhan, S. A. Senawi, A. Mardhiah

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Studies on Samarium doped glasses possess lot of interest due to their potential applications for high-density optical memory, optical communication device, the design of laser and color display etc. Sm3+ doped borotellurite glasses of the system (70-x) TeO2-20B2O3-10ZnO-xSm2O3 (where x = 0.0, 0.5, 1.0, 1.5, 2.0 and 2.5 mol%) have been prepared using melt-quenching method. Their physical properties such as density, molar volume and oxygen packing density as well as the optical measurements by mean of their absorption and emission characteristic have been carried out at room temperature using UV/VIS and photoluminescence spectrophotometer. The results of physical properties are found to vary with respect to Sm3+ ions content. Meanwhile, three strong absorption peaks are observed and are well resolved in the ultra violet and visible regions due to transitions between the ground state and various excited state of Sm3+ ions. Thus, the photoluminescence spectra exhibit four emission bands from the initial state, which correspond to the 4G5/2 → 6H5/2, 4G5/2 → 6H7/2, 4G5/2 → 6H9/2 and 4G5/2 → 6H11/2 fluorescence transitions at 562 nm, 599 nm, 645 nm and 706 nm respectively.

Keywords: absorption, borotellurite, down-conversion, emission

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Authors: M. Koksal, T. Ozyazici, E. Gurdal, M. Yarım, E. Demirpolat, M. B. Y. Aycan

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The discovery of new drugs in cancer chemotherapy is still a major topic because of severe side effects, selectivity problems and resistance development potential of existing drugs. In recent years, combined anticancer therapies or multi-acting drugs are clinically preferred over traditional cytotoxic treatment, with the aim of avoiding resistance and toxic side effects. Arrangement of multi-acting targets can be carried out either by combination of several drugs with different mechanisms or by usage of a single chemical compound capable of regulating several targets of a disease with multiple factors. In literature, several pyrimidine and piperazine derivatives have been involved in the structure of many compounds which have been used as chemotherapeutic agents along with wide clinical applications. The aim of this study is to combine pyrimidine and piperazine core structures to research and develop novel piperazinylpyrimidine derivatives with selective cytotoxicity over cancer cells. In this study, a group of novel 6-fluorophenyl-3-[2-(substitutedpiperazinyl)ethyl] hexahydropyrimidine-2,4-dione derivatives designed to observe the desired anticancer activity due to pyrimidine and piperazine based scaffolds. Target compounds were obtained by the reaction of appropriate piperazine derivatives and 6-(2/4-fluorophenyl)-3-(2-chloroethyl)hexahydropyrimidine-2,4-dione. The synthetic pathway of 6-(2/4-fluorophenyl)-3-(2-chloroethyl)hexahydropyrimidine-2,4-dione was started with Rodionov reaction using aldehyde, malonic acid and ammonium acetate in ethanol. Isolated β-fluorophenyl-β-amino acids were treated with 2-chloroethylisocyanate in the presence of an aqueous sodium hydroxide solution at room temperature to yield the sodium salts of the corresponding ureido acids. By addition of a mineral acid, ureido acids were precipitated. Later, these ureido acids were refluxed in thionyl chloride to give the 6-(2/4-fluorophenyl)-3-(2-chloroethyl)hexahydropyrimidine-2,4-di-one which were furthermore treated with secondary amines. Structures of purified compounds were characterized with IR, 1H-NMR, 13C-NMR, mass spectroscopies and elemental analysis. All of the compounds gave satisfactory analytical and spectroscopic data, which were in full accordance with their depicted structures. In IR spectra of the compounds, N-H group was seen at 3230-3213 cm⁻¹. C-H was seen at 3100-2820 cm⁻¹ and C=O vibrational peaks were observed approximately at 1725 and 1665 cm⁻¹ in accordance with literature. In the NMR spectra of target compounds, the methylene protons of piperazine give two separate multiplet peaks around 3.5 and 4.5 ppm representing the successful N-alkylation of the structure. The cytotoxic activity of the synthesized compounds was investigated on human bronchial epithelial (BEAS 2B), lung (A549), colon adenocarcinoma (COLO205) and breast (MCF7) cell lines, by means of sulphorhodamine B (SRB) assays in triplicate. IC₅₀ values of the screened derivatives were found in range of 11.8-78 µM. This project was supported by The Scientific and Technological Research Council of Turkey (TUBITAK, Project no: 215S157).

Keywords: cytotoxicity, hexahydropyrimidine, piperazine, sulphorhodamine B assay

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Authors: Sachin Mahajan, Ghizal Ansari

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TeO2-WO3-Li2O glass doped erbium ions (1mol %) and embedded silver nanoparticles( Ag NPs) has successfully been prepared by melt quenching technique and increasing the heat-treatment duration. The amorphous nature of the glass is determined by X-ray diffraction method, and the presences of silver nanoparticles are confirmed using Transmission Electron Microscopy analysis. TEM image reveals that the Ag NPs are dispersed homogeneously with average size 18 nm. From the UV-Vis absorption spectra, the surface plasmon resonance (SPR) peaks are detected at 550 and 578 nm. Under 980 nm excitation wavelengths, enhancement of red upconversion fluorescence and near-infrared broadband emission around 1550nm of Er3+ ions doped tellurite glasses containing Ag NPs have been observed. The observed enhancement of Er3+ emission is mainly attributed to the local field effects of Ag NPs causes an intensified electromagnetic field around NPs. For observed enhancement involved mechanisms are discussed.

Keywords: erbium ions, silver nanoparticle, surface plasmon resonance, upconversion emission

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Authors: Nesrine T. Lamie

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Four, accurate, precise, and sensitive spectrophotometric methods are developed for the simultaneous determination of a binary mixture containing amlodipine besylate (AM) and atenolol (AT) where AM is determined at its λmax 360 nm (0D), while atenolol can be determined by different methods. Method (A) is absorpotion factor (AFM). Method (B) is the new Ratio Difference method(RD) which measures the difference in amplitudes between 210 and 226 nm of ratio spectrum., Method (C) is novel constant center spectrophotometric method (CC) Method (D) is mean centering of the ratio spectra (MCR) at 284 nm. The calibration curve is linear over the concentration range of 10–80 and 4–40 μg/ml for AM and AT, respectively. These methods are tested by analyzing synthetic mixtures of the cited drugs and they are applied to their commercial pharmaceutical preparation. The validity of results was assessed by applying standard addition technique. The results obtained were found to agree statistically with those obtained by a reported method, showing no significant difference with respect to accuracy and precision.

Keywords: amlodipine, atenolol, absorption factor, constant center, mean centering, ratio difference

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Authors: Seyed Mahdi Rafiaei

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In this investigation, red emitting Eu³⁺ doped YVO₄ nano-phosphors have been synthesized via the facile combustion method using isobutyl nitrite and urea fuels, individually. Field-emission scanning electron microscope (FE-SEM) images, high resolution transmission electron microscope (TEM) images and X-ray diffraction (XRD) spectra reveal that the mentioned fuels can be used successfully to synthesis YVO₄: Eu³⁺ nano-particles. Interestingly, the fuels have a large effect on the size and morphology of nano-phosphors as well as luminescence properties. Noteworthy the use of isobutyl nitrite provides an average particle size of 65 nm, while the employment of urea, results in the formation of larger particles and also provides higher photoluminescence emission intensity. The improved luminescence performance is attributed to the condition of chemical reaction via the combustion synthesis and the size of synthesized phosphors.

Keywords: phosphors, combustion, fuels, luminescence, nanostructure

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Authors: Ravinesh C. Deo

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This article reviews the role of nozzle-exit conditions on the flow field of a plane jet. The jet issuing from a sharp-edged orifice plate at a Reynolds number (Re=18000) with nozzle aspect ratio (AR=72) exhibits the greatest shear-layer instabilities, highest entrainment and jet-spreading rates compared to the radially contoured nozzle. The growth rate of the shear-layer is the highest for the orifice-jet although this property could be amplified for larger Re or AR. A local peak in turbulent energy is found at x=10h. The peak appears to be elevated for an orifice-jet with lower Re or AR. The far-field energy sustained by the orifice-jet exceeds the contoured case although a higher Re and AR may enhance this value. The spectra displays the largest eddies generated by the contoured nozzle. However, the frequency of coherent eddies is higher for the orifice-jet, with a larger magnitude achievable for lower Re and AR.

Keywords: plane jet, Reynolds number, nozzle-exit conditions, nozzle geometry, aspect ratio

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Authors: Lijuan Li

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Nitric oxide (NO) has become a fascinating entity in biological chemistry over the past few years. It is a gaseous lipophilic radical molecule that plays important roles in several physiological and pathophysiological processes in mammals, including activating the immune response, serving as a neurotransmitter, regulating the cardiovascular system, and acting as an endothelium-derived relaxing factor. NO functions in eukaryotes both as a signal molecule at nanomolar concentrations and as a cytotoxic agent at micromolar concentrations. The latter arises from the ability of NO to react readily with a variety of cellular targets leading to thiol S-nitrosation, amino acid N-nitrosation, and nitrosative DNA damage. Nitric oxide can readily bind to metals to give metal-nitrosyl (M-NO) complexes. Some of these species are known to play roles in biological NO storage and transport. These complexes have different biological, photochemical, or spectroscopic properties due to distinctive structural features. These recent discoveries have spawned a great interest in the development of transition metal complexes containing NO, particularly its iron complexes that are central to the role of nitric oxide in the body. Spectroscopic evidence would appear to implicate species of “Fe(NO)2+” type in a variety of processes ranging from polymerization, carcinogenesis, to nitric oxide stores. Our research focuses on isolation and structural studies of non-heme iron nitrosyls that mimic biologically active compounds and can potentially be used for anticancer drug therapy. We have shown that reactions between Fe(NO)2(CO)2 and a series of imidazoles generated new non-heme iron nitrosyls of the form Fe(NO)2(L)2 [L = imidazole, 1-methylimidazole, 4-methylimidazole, benzimidazole, 5,6-dimethylbenzimidazole, and L-histidine] and a tetrameric cluster of [Fe(NO)2(L)]4 (L=Im, 4-MeIm, BzIm, and Me2BzIm), resulted from the interactions of Fe(NO)2 with a series of substituted imidazoles was prepared. Recently, a series of sulfur bridged iron di nitrosyl complexes with the general formula of [Fe(µ-RS)(NO)2]2 (R = n-Pr, t-Bu, 6-methyl-2-pyridyl, and 4,6-dimethyl-2-pyrimidyl), were synthesized by the reaction of Fe(NO)2(CO)2 with thiols or thiolates. Their structures and properties were studied by IR, UV-vis, 1H-NMR, EPR, electrochemistry, X-ray diffraction analysis and DFT calculations. IR spectra of these complexes display one weak and two strong NO stretching frequencies (νNO) in solution, but only two strong νNO in solid. DFT calculations suggest that two spatial isomers of these complexes bear 3 Kcal energy difference in solution. The paramagnetic complexes [Fe2(µ-RS)2(NO)4]-, have also been investigated by EPR spectroscopy. Interestingly, the EPR spectra of complexes exhibit an isotropic signal of g = 1.998 - 2.004 without hyperfine splitting. The observations are consistent with the results of calculations, which reveal that the unpaired electron dominantly delocalize over the two sulfur and two iron atoms. The difference of the g values between the reduced form of iron-sulfur clusters and the typical monomeric di nitrosyl iron complexes is explained, for the first time, by of the difference in unpaired electron distributions between the two types of complexes, which provides the theoretical basis for the use of g value as a spectroscopic tool to differentiate these biologically active complexes.

Keywords: di nitrosyl iron complex, metal nitrosyl, non-heme iron, nitric oxide

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Authors: Kriengsak Damampai, Skulrat Pichaiyut, Amit Das, Charoen Nacason

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The curing of epoxidized natural rubber (ENR) was performed by using metal ions (Ferric chloride, FeCl₃). Two different mole% of epoxide were used there are 25 mole% (ENR-25) and 50 mole% (ENR-50) epoxizied natural rubber. The main aim of this work was investigated the influence of metal ions on the coordination reaction of epoxidized natural rubber. Also, cure characteristics and mechanical properties of the rubber compounds were investigated. It was found that the ENR-50 compounds indicated superior modulus and tensile strength than the ENR-25 compounds. This was attributed to higher the cross-linking in the rubber via coordination linkages between the oxidation groups in ENR molecule and FeCl₃of metal ions. Various quantities of FeCl3 were also investigated. It is seen that the ENR-25 and 50 mole% compounds with FeCl₃ of more than 3 mmol exhibited higher modulus and tensile strength compare to the pure ENR. Furthermore, the FTIR spectra was used to confirm the cross-linked of ENR with FeCl₃.

Keywords: Epoxidized natural rubber, Ferric chloride, cross-linking, Coordination

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Authors: Ayodele Odularu, Peter Ajibade, Albert Bolhuis

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This study aimed at assessing the antibacterial activities of four zinc (II) complexes. Zinc (II) complexes of nitrogen, oxygen and sulfur coordination modes were synthesized using direct substitution reaction. The characterization techniques involved physicochemical properties (molar conductivity) and spectroscopic techniques. The molar conductivity gave the non-electrolytic nature of zinc (II) complexes. The spectral studies of zinc (II) complexes were done using electronic spectra (UV-Vis) and Fourier Transform Infra-red Spectroscopy (FT-IR). Spectral data from the spectroscopic studies confirmed the coordination of the mixed ligands with zinc (II) ion. The antibacterial activities of zinc(II) complexes of were all in supportive of Overtone’s concept and Tweedy’s theory of chelation for bacterial strains of S. aureus MRSA252 and E coli MC4100 because the zones of inhibition were greater than the corresponding ligands. In summary, all zinc (II) complexes of ZEPY, ZE1PH, ZE1PY and ZE135PY all have potentials for antibacterial activities.

Keywords: antibacterial activities, spectral studies, syntheses, zinc(II) complexes

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Authors: Juan Xia, Jiaxu Yan, Ze Xiang Shen

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The tuneable interlayer interactions in two-dimensional (2D) transition metal dichlcogenides (TMDs) offer an exciting platform for exploring new physics and applications by material variety, thickness, stacking sequence, electromagnetic filed, and stress/strain. Compared with the five methods mentioned above, high pressure is a clean and powerful tool to induce dramatic changes in lattice parameters and physical properties for 2D TMD materials. For instance, high pressure can strengthen the van der Waals interactions along c-axis and shorten the covalent bonds in atomic plane, leading to the typical first-order structural transition (2Hc to 2Ha for MoS2), or metallization. In particular, in the case of WTe₂, its unique symmetry endows the significant anisotropy and the corresponding unexpected properties including the giant magnetoresistance, pressure-induced superconductivity and Weyl semimetal states. Upon increasing pressure, the Raman peaks for WTe₂ at ~120 cm⁻¹, are gradually red-shifted and totally suppressed above 10 GPa, attributed to the possible structural instability of orthorhombic Td phase under high pressure and phase transition to a new monoclinic T' phase with inversion symmetry. Distinct electronic structures near Fermi level between the Td and T' phases may pave a feasible way to achieve the Weyl state tuning in one material without doping.

Keywords: 2D TMDs, electronic property, high pressure, first-principles calculations

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Authors: Hua Jin, Il Kim

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The biocompatible tadpole-shaped polypeptides with one cyclic polypeptides ring and two alkyl chain tails were synthesized by N-heterocyclic carbine (NHC)-mediated ring-opening polymerization (ROP) of α-amino acid N-carboxyanhydrides (NCAs). First, the NHC precursor, denoted as [NHC(H)][HCO₃], with two alkyl chains at the nitrogen was prepared by a simple anion metathesis of imidazole(in)ium chlorides with KHCO₃. Then NHC releasing from the [NHC(H)][HCO₃] directly initiated the ROP of NCA to produce the cyclic polypeptides. Finally, the tadpole-shaped polypeptides with two regulable tails were obtained. The target polypeptides were characterized by nuclear magnetic resonance spectrum (1H NMR), Fourier transform infrared spectroscopy (FT-IR), gel permeation chromatography (GPC) and matrix-assisted laser desorption ionization-time of flight mass spectra (MALDI-TOF MS). This pioneering approach simplifies the synthesis procedures of tadpole-shaped polypeptides compared to other methods, which usually requires specific intramolecular ring-closure reaction.

Keywords: cyclic polypeptides, α-amino acid N-carboxyanhydrides, N-heterocyclic carbene, ring-opening polymerization, tadpole-shaped

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Authors: Jinghui Peng, Shanyu Tang, Jia Li

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Steganalysis seeks to detect the presence of secret data embedded in cover objects, and there is an imminent demand to detect hidden messages in streaming media. This paper shows how a steganalysis algorithm based on Fast Fourier Transform (FFT) can be used to detect the existence of secret data embedded in streaming media. The proposed algorithm uses machine parameter characteristics and a network sniffer to determine whether the Internet traffic contains streaming channels. The detected streaming data is then transferred from the time domain to the frequency domain through FFT. The distributions of power spectra in the frequency domain between original VoIP streams and stego VoIP streams are compared in turn using t-test, achieving the p-value of 7.5686E-176 which is below the threshold. The results indicate that the proposed FFT-based steganalysis algorithm is effective in detecting the secret data embedded in VoIP streaming media.

Keywords: steganalysis, security, Fast Fourier Transform, streaming media

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Authors: Chaoyan Huang, Hongxia Zheng

Abstract:

For deep space exploration and long duration interplanetary manned missions, protection of astronauts from cosmic radiation is an unavoidable problem. However, passive shielding can be little effective for protecting particles which energies are greater than 1GeV/nucleon. In this study, active magnetic protection method is adopted. Taking into account the structure and size of the end-cap, eight shielding magnetic field configurations are designed based on the Hoffman configuration. The shielding effect of shielding magnetic field structure, intensity B and thickness L on H particles with 2GeV energy is compared by test particle simulation. The result shows that the shielding effect is better with the linear type magnetic field structure in the end-cap region. Furthermore, two magnetic field configurations with better shielding effect are investigated through H and He galactic cosmic spectra. And the shielding effect of the linear type configuration adopted in the barrel and end-cap regions is best.

Keywords: galactic cosmic rays, active protection, shielding magnetic field configuration, shielding effect

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Authors: L. Srikanth, D. Neelima Satyam

Abstract:

The transmission line towers are one of the important life line structures in the distribution of power from the source to the various places for several purposes. The predominant external loads which act on these towers are wind and earthquake loads. In this present study tower is analyzed using Indian Standards IS: 875:1987 (Wind Load), IS: 802:1995 (Structural Steel), IS:1893:2002 (Earthquake) and dynamic analysis of tower has been performed considering ground motion of 2001 Bhuj Earthquake (India). The dynamic analysis was performed considering a tower system consisting two towers spaced 800m apart and 35m height each. This analysis has been performed using numerical time stepping finite difference method which is central difference method were employed by a developed MATLAB program to get the normalized ground motion parameters includes acceleration, frequency, velocity which are important in designing the tower. The tower is analyzed using response spectrum analysis.

Keywords: response spectra, dynamic analysis, central difference method, transmission tower

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

Abstract:

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

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

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Authors: Sani Abubakar, Oumar Al-Mubarak Adoum

Abstract:

The leaves extracts of Cassia sieberiana D. C. were screened for antimicrobial bioassay against Staphylococcus aureus, Salmonella typhi, and Escherichia coli and cytotoxicity using Brine Shrimp Test (BST). The crude ethanol extract, Chloroform soluble fraction, aqueous soluble fraction, ethyl acetate soluble fraction, methanol soluble fraction, and n-hexane soluble fraction were tested against antimicrobial and cytotoxicity. The Ethyl acetate fraction obtained proved to be most active in inducing complete lethality at minimum doses in BST and also active on Salmonella typhi. The bioactivity result was used to guide the column chromatography, which led to the isolation of pure compound CSB-8, which was found active in the BST with an LC₅₀ value of 34(722-182)µg/ml and showed remarkable activity on Salmonella typhi (zone of inhibition 25mm) at 10,000µg/ml. The ¹H-NMR, ¹³C NMR, FTIR, and GC-MS spectra of the compound suggested the proposed structure to be 2-pentadecanone.

Keywords: antimicrobial bioassay, cytotoxicity, column chromatagraphy, Cassia sieberiana D.C.

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Authors: Snehal L. Kadam, Shriniwas B. Kulkarni

Abstract:

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

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

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Authors: S. V. Patil , S. K. Sahoo, K. Y. Chougule, S. S. Patil

Abstract:

Spherically agglomerated crystals of Pioglitazone hydrochloride (PGH) with improved flowability and compactibility were successfully prepared by emulsion solvent diffusion method. Plane agglomerates and agglomerates with additives: polyethylene glycol 6000 (PEG), polyvinyl pyrrolidone (PVP) and β cyclodextrin (β-CD) were prepared using methanol, chloroform and water as good solvent, bridging liquid and poor solvent respectively. Particle size, flowability, compactibility and packability of plane, PEG and β-CD agglomerates were preferably improved for direct tableting compared with raw crystals and PVP agglomerates of PGH. These improved properties of spherically agglomerated crystals were due to their large and spherical shape and enhanced fragmentation during compaction which was well supported by increased tensile strength and less elastic recovery of its compact. X-ray powder diffraction and differential scanning calorimetry study were indicated polymorphic transition of PGH from form II to I during recrystallization but not associated with chemical transition indicated by fourier transforms infrared spectra.

Keywords: spherical crystallization, pioglitazone hydrochloride, compactibility, packability

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

Abstract:

Herein, we reported the influence of La³⁺ substitution on structural, magnetic and dielectric properties of CoFe₂O₄ nanoparticles synthesized by starch-assisted sol-gel combustion method. X-ray diffraction pattern confirmed the formation of cubic spinel structure of La³⁺ ions doped CoFe₂O₄ nanoparticles. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of La³⁺ substituted CoFe₂O₄ nanoparticles. The field emission scanning electron microscopy study revealed that La³⁺ substituted CoFe2O4 nanoparticles were in the range of 10-40 nm. The magnetic properties of La³⁺ substituted CoFe₂O₄ nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with La³⁺ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied with change of concentration of La³⁺ ions in CoFe₂O₄ nanoparticles. The variation in optical properties was studied via UV-Vis absorption spectroscopy. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: starch, sol-gel combustion method, nanoparticles, magnetic properties, dielectric properties

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