Sucrose chelated auto combustion synthesis of BiFeO3 nanoparticles: Magnetically recoverable catalyst for the one‐pot synthesis of polyhydroquinoline

Sucrose chelated Bismuth ferrite (BiFeO₃) nanoparticles as a novel heterogeneous catalyst was synthesized by an auto combustion route. Different calcination temperatures (150 °C, 450 °C, 550 °C, 650 °C, 750 °C and 850 °C) have been employed to obtain single phased BiFeO₃ nanoparticles. The perovskite structure formation and disappearance of organic phase (sucrose) was obtained by Fourier transform infrared spectroscopy (FT‐IR). Phase determination and structural characterization was carried out by powder X‐ray diffraction (XRD). The magnetic properties were analyzed by vibrating sample magnetometer (VSM) whereas surface area/pore volume was obtained by Brunauer–Emmett–Teller (BET). Transmission electron microscope (TEM) analyzed the particles size and morphology. Thermal stability was investigated by thermogravimetric analysis (TGA) and determination of constituent elements was carried out by X‐ray Photo‐Electron Spectroscopy (XPS). Raman spectroscopy confirmed the perovskite structure of the synthesized materials. The BiFeO₃ nanoparticles so obtained were employed as heterogeneous catalyst for the synthesis of polyhydroquinoline derivatives. All the polyhydroquinoline derivatives were characterized by Fourier transform infrared spectroscopy (FT‐IR) and Nuclear magnetic resonance spectroscopy (¹H NMR). For the very first time ever we have used BiFeO₃ as a recyclable magnetic nanocatalyst in the one‐pot four component cyclization reaction of benzaldehyde, ethylacetoacetate/methylacetoacetate, dimedone/cyclohexane‐1,3‐dione, and ammonium acetate for the synthesis of polyhydroquinoline derivatives without solvent under refluxing conditions to provide excellent yields of products. BiFeO₃ nanocatalyst (without any functionalization/surface coatings) shows easy magnetic separation, recyclability, reusability along with excellent yield of polyhydroquinoline derivatives in an economic and benign way.     

Effect of environmental temperature and applied potential on water desalination performance using electrodialysis

Desalination of brackish water is a challenging task for higher recovery of water. In most of the cases, water recovery is low with high wastage. Electrodialysis (ED) provides a solution of water desalination with high recovery. Ion-exchange membranes are the main component for electrodialysis system. Here cation-exchange membrane and anion-exchange membrane were synthesized by free-radical polymerization for water desalination by ED. ATR-FTIR confirms the successful functionalization of the membranes and scanning electron microscopy technique reveals the dense morphology of the membranes. Here we used polyethylene as a binder and blow film extrusion for film formation, which is not only economically viable as well as large amount of membranes can be produced without using hazardous solvent. The desalination study reveals the improvement in desalination performance with slight increment in temperature which may be due to higher ionic mobility. The mechanical and thermal stability of the membranes was characterized to ensure the viability of membranes for desalination at higher temperatures. Effect of applied potential was also studied in the removal of pathogens during desalination and confirmed that 2 V/cell pair applied potential removes almost 97% pathogens during desalination in continuous mode.     

RP–LC Simultaneous Determination of Aconitine,Solanine and Piperine in an Ayurvedic Medicine

By optimizing the extraction, separation and analytical conditions, a reliable, rapid, simple and accurate liquid chromatography method with UV detection was developed for the simultaneous quantitative determination of aconitine, solanine and piperine in an ayurvedic preparation prepared from Aconitum ferox, Solanum indicum, Piper nigrum and Piper longum. The separation of these alkaloids was achieved on an reversed phase C-18 column (250 mm × 4.6 mm ID, 5 μm particle size), with isocratic elution using a mixture of acetonitrile–potassium hydrogen phosphate buffer (10 mM, pH 7.5)–methanol (60:25:15, v/v) at a flow rate of 1 mL min⁻¹ with UV detection at 227 nm for aconitine and solanine while 343 nm for piperine. The calibration curves were linear with correlation coefficients of 0.9990, 0.9942, 0.9989 for solanine, piperine and aconitine, respectively. The % Relative standard deviation (%RSD) values were less than 2% in the concentration range of 10–100 μg mL⁻¹ for all the three alkaloids. Intra-day assay and inter-day assay precision of the analytes were less than 2%, and the average recovery rates obtained were in the range of 98–102% for all with %RSD below 2%. Quantitative analysis of the alkaloids in the laboratory and marketed formulations showed that the contents of the alkaloids varied significantly. This method can provide a scientific and technical platform to the product manufacturers for setting up a quality control standard as well as to the public for quality and safety assurance of the proprietary ayurvedic formulations.

     

Ferrocenyl-nitrogen donor ligands. Synthesis and characterization of rhodium(I) complexes of ferrocenylpyridine and related ligands

The preparation of a series of complexes of the types [RhCl(CO)₂(L)], [RhCl(cod)(L)] and [Rh(cod)(L)₂]ClO₄, where L is a ligand incorporating a ferrocenyl group and a pyridine ring is described. Complexes were characterized using NMR, IR and electronic spectroscopy. The electrochemical behaviour of the complexes was examined using cyclic voltammetry. The X-ray structures of three of the complexes, [RhCl(CO)₂{NC₅H₄CNC₆H₄(η⁵-C₅H₄)Fe(η⁵-C₅H₅)}], [RhCl(cod)(3-Fcpy)] and [RhCl(cod){3-Fc(C₆H₄)py}], were determined.     

UV Excited‐State Photoresponse of Biochromophore Negative Ions

Members of the green fluorescent protein (GFP) family may undergo irreversible phototransformation upon irradiation with UV light. This provides clear evidence for the importance of the higher‐energy photophysics of the chromophore, which remains essentially unexplored. By using time‐resolved action and photoelectron spectroscopy together with high‐level electronic structure theory, we directly probe and identify higher electronically excited singlet states of the isolated para‐ and meta‐chromophore anions of GFP. These molecular resonances are found to serve as a doorway for very efficient electron detachment in the gas phase. Inside the protein, this band is found to be resonant with the quasicontinuum of a solvated electron, thus enhancing electron transfer from the GFP to the solvent. This suggests a photophysical pathway for photoconversion of the protein, where GFP resonant photooxidation in solution triggers radical redox reactions inside these proteins.     

Investigating structural aspects to understand the putative/claimed non‐toxicity of the Hg‐based Ayurvedic drug Rasasindura using XAFS

XANES‐ and EXAFS‐based analysis of the Ayurvedic Hg‐based nano‐drug Rasasindura has been performed to seek evidence of its non‐toxicity. Rasasindura is determined to be composed of single‐phase α‐HgS nanoparticles (size ～24 nm), free of Hg⁰ or organic molecules; its structure is determined to be robust (<3% defects). The non‐existence of Hg⁰ implies the absence of Hg‐based toxicity and establishes that chemical form, rather than content of heavy metals, is the correct parameter for evaluating the toxicity in these drugs. The stable α‐HgS form (strong Hg—S covalent bond and robust particle character) ensures the integrity of the drug during delivery and prevention of its reduction to Hg⁰ within the human body. Further, these comparative studies establish that structural parameters (size dispersion, coordination configuration) are better controlled in Rasasindura. This places the Ayurvedic synthesis method on par with contemporary techniques of nanoparticle synthesis.     

Bandwidth enhancement of transformation optics-based cloak with reduced parameters

In this paper, dispersive cloak design with broad bandwidth and minimal scattering cross section is proposed by appropriately selecting a radial permeability for each shell in a discretized reduced cloak. The dispersive medium is constructed by artificially varying the inner radius of the cloak with frequency, and this variation results into unique material properties at every frequency. The variation of inner radius of the cloak with frequency is artificial since the actual physical dimension of inner radius remains invariant. The relation between bandwidth and geometrical parameters of cloak is obtained by ensuring that transformation media must satisfy the condition that group velocity must remain less than the speed of light along every direction for a finite frequency range. The proposed cloak provides \(8.9\,\%\) bandwidth with respect to the center frequency for \(50\,\%\) reduction in total scattering cross section, and at the design frequency, the minimum scattering cross section obtained is \(0.266\). The proposed dispersive cloak design is verified by numerical full-wave simulations results which also confirm good cloaking performance.     

Design and synthesis of coordination networks containing amide,pyridine and carboxylate functionalities

The reactions of bis(pyridinecarboxamido)alkane with copper(II) in the presence of mono or dicarboxylic acids resulted in discrete species, one-dimensional and two-dimensional networks. The carboxylates considered for this study include m-nitrobenzoic acid, isophthalic acid and succinic acid. In the presence of m-nitrobenzoic acid the ligands with Cu(II) form 1D coordination networks which include m-nitrobenzoic acid and water molecules as guests. The use of isophthalic acid resulted in discrete species while the use of succinic acid resulted in a two-dimensional layer containing rectangular grids of dimension 9.7 × 16.5 Å². The 2D layers in this complex exhibit inclined 2-fold interpenetration. Further, all these coordination networks are assembled via hydrogen bonding interactions between the amides and water molecules. The Cu(II) centre exhibits a unique octahedral coordination geometry, for the complexes reported here, as it coordinates with two each of pyridine moieties, water molecules and carboxylates.     

Crosslinked styrene‐maleic acid copolymer complexes of some transition metals and their adsorption behavior

Transition metal complexes of linear and crosslinked styrene‐maleic acid copolymer were prepared in ethyl alcohol. The complexes appear as micro clusters fairly uniformly distributed in the copolymer matrix. Vapor adsorption–desorption studies of the complex beads with methyl isobutyl ketone (MIBK), toluene and ethyl alcohol show initial fast release followed by a steady and slow release. Hydrogen adsorption at room temperature was studied for a few complexes up to about 650 torr, which showed initial slow adsorption followed by a rapid increase at about 550 torr. Copyright © 2005 John Wiley & Sons, Ltd.