<Emphasis Type="Italic">Bis</Emphasis>(macrocyclic)dinickel(II) complexes containing phenylene bridges between 13-membered triaza dioxa macrocyclic ligands: <Emphasis Type="Italic">in-situ</Emphasis> one pot template synthesis,characterization and catalytic oxidation of cyclohexene

A new series of bis(macrocyclic)dinickel(II) complexes containing phenylene bridges between 13-membered triaza dioxa macrocyclic subunits have been synthesized via in-situ One Pot Template Condensation (IOPTC) of nitrogen–nitrogen linker, CH₂O and 1,8-diamino-3,6-dioxaoctane and nickel(II) in a 1:4:2:2 molar ratio. These complexes have been found to be effective catalysts for the selective oxidation of cyclohexene to 2-cyclohexene-1-one and 2-cyclohexene-2-ol with molecular oxygen as the oxidant.     

Selective determination of penicillamine by on-line vapor-phase generation combined with Fourier transform infrared spectrometry

In this work, an on-line system with vapor-phase generation (VPG) and Fourier transform infrared (FTIR) spectrometric detection has been developed as a direct and highly selective analytical technique for the assay of penicillamine (PA). Potassium iodate solution was injected into a reactor, heated at 75 °C, containing PA. The CO generated under these conditions was transported by means of N₂ gas carrier stream to an infrared gas cell and corresponding FTIR spectra were acquired in a continuous mode. The maximum absorbance of CO band at 2170 cm⁻¹, corrected by a baseline established between 2240 and 2000 cm⁻¹ at a nominal resolution of 2 cm⁻¹, was selected as a measurement criterion. Initially, the effect of different chemical, physical and spectroscopic parameters, such as concentration and volume of oxidant, pH, equilibrium time, reactor temperature, reactor volume, N₂ carrier flow rate and number of scans on the analytical signals were evaluated by using a short path length (10 cm) IR gas cell. At optimum experimental conditions, the method provided a relatively broad linear dynamic range of 4-380 mg L⁻¹, a limit of detection of 0.5 mg L⁻¹, a sampling frequency of 15 h⁻¹ and a relative standard deviation (R.S.D.) of 1.6%. Further, the method was successfully applied to the determination of PA in pharmaceutical formulations and results compared well with those obtained by a reference colorimetric method.     

Further properties of Azimi-Hagler banach spaces

For the Azimi-Hagler spaces more geometric and topological properties are investigated. Any constructed space is denoted by X _α,p . We show

Large-eddy simulation of evaporating spray in a coaxial combustor

Large-eddy simulation of an evaporating isopropyl alcohol spray in a coaxial combustor is performed. The Favre-averaged, variable density, low-Mach number Navier-Stokes equations are solved on unstructured grids with dynamic subgrid scale model to compute the turbulent gas-phase. The original incompressible flow algorithm for LES on unstructured grids by [Mahesh et al., J. Comp. Phys. 197 (2004) 215–240] is extended to include density variations and droplet evaporation. An efficient particle-tracking scheme on unstructured meshes is developed to compute the dispersed phase. Experimentally measured droplet size distribution and size-velocity correlation near the nozzle exit are used as the inlet conditions for the spray. The predictive capability of the LES approach on unstructured grids together with Lagrangian droplet dynamics models to capture the droplet dispersion characteristics, size distributions, and the spray evolution is examined in detail. The mean and turbulent quantities for the gas and particle phases are compared to experimental data to show good agreement. It is shown that for low evaporation rates considered in the present study, a well resolved large-eddy simulation together with simple subgrid models for droplet evaporation and motion provides good agreement of the mean and turbulent quantities for the gas and droplet phases compared to the experimental data. This work represents an important first step to assess the predictive capability of the unstructured grid LES approach applied to spray vaporization. The novelty of the results presented is that they establish a baseline fidelity in the ability to simulate complex flows on unstructured grids at conditions representative of gas-turbine combustors.     

Salt‐assisted liquid–liquid extraction in microchannel

In this study, for the first time, salt‐assisted liquid–liquid extraction was performed in a microchannel system. The proposed design is based on the increase of contact surface area between target analytes and extracting phase during the sample and extracting phase transfer in microchannel. In this method, first sample solution, extracting solvent, and salt were mixed by stirrer and simultaneously delivered into a microchannel using a syringe pump. In order to optimize the influential parameters on the extraction efficiency of the proposed method, zidovudine and tenofovir disoproxil fumarate were selected as model analytes. The main parameters such as extracting solvent and its volume, salt amount, pH of sample solution, and microchannel shape, length, and its inner diameter were investigated and optimized. Under the optimized conditions, the proposed method was linear in the range of 0.1–30 µg/mL and R² coefficients were equal to 0.9922 and 0.9947 for zidovudine and tenofovir disoproxil fumarate, respectively. Extraction efficiency of the proposed method was compared with conventional salt‐assisted liquid–liquid extraction. The results show that the proposed design has higher extraction efficiency than conventional salt‐assisted liquid–liquid extraction. Finally, the proposed method was successfully applied for the determination of zidovudine and tenofovir disoproxil fumarate in plasma samples.     

Two-dimensional self-assembly of 1-pyrylphosphonic acid: transfer of stacks on structured surface

Strong hydrogen bonding and pi-pi stacking between 1-pyrylphosphonic acid (PYPA) molecules were exploited to create self-assembled two-dimensional supramolecular structures. Polycrystalline films of these laminate crystalline PYPA bilayers were easily deposited onto the solid supports through a simple spin-coating technique. Atomic force microscopy (AFM), scanning tunneling microscopy (STM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption, and fluorescence spectroscopy reveal that processing parameters, such as solvent, concentration, and surface of the substrate, are critical factors in determining the final morphology of the stacked film. Robust laminate structures could be obtained only when short alkyl chain protic solvents (methanol or ethanol) and a nonhydrophobic substrate surface were used. Polycrystalline films were formed through the nucleation and growth of PYPA molecules into laminate structures at the air/solvent interface before they land on the substrate during the spin-coating process. These films possess good mechanical properties and were easily transferred onto a SiO2/Si substrate that was patterned with Au electrodes without breaking their crystalline structures. The successful transfer of the laminate crystals allows us to probe their electrical properties through a field effect transistor device. A gating effect on the charge transport of the stacked films indicates that PYPA laminate crystal possesses p-typed semiconductor characteristics.     

Studies on photocatalytic performance and photodegradation kinetics of zinc oxide nanoparticles prepared by microwave-assisted sol–gel technique using ethylene glycol

ZnO nanoparticles with an average particle size of 27 nm were fabricated using a microwave-assisted sol–gel method in the presence of ethylene glycol. The nanoparticles were characterized by X-ray diffraction, Monshi’s equation, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy. The band gap energy of the nanoparticles was measured to be 3.27 eV by UV–Vis absorption and reflection spectroscopy. Photocatalytic activity of the synthesized nanoparticles was assessed by degrading nitrophenol in aqueous solution under UV-C irradiation. The effects of initial nitrophenol concentration, amount of photocatalyst, and of pH on the photodegradation process were investigated. Degradation samples were analyzed by UV–Vis spectroscopy. Nitrophenol was removed by 98 % within 240 min. The degradation kinetics were studied and fitted well to pseudo-first-order and Langmuir–Hinshelwood models.