Microwave synthesis of magnetic Fe3O4 nanoparticles used as a precursor of nanocomposites and ferrofluids

Methods to synthesize magnetic Fe₃O₄ nanoparticles and to modify the surface of particles are presented in the present investigation. Fe₃O₄ magnetic nanoparticles were prepared by the co-precipitation of Fe³⁺ and Fe²⁺, NH₃·H₂O was used as the precipitating agent to adjust the pH value, and the aging of Fe₃O₄ magnetic nanoparticles was accelerated by microwave (MW) irradiation. The obtained Fe₃O₄ magnetic nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and vibrating sample magnetometer (VSM). The average size of Fe₃O₄ crystallites was found to be around 8–9 nm. Thereafter, the surface of Fe₃O₄ magnetic nanoparticles was modified by stearic acid. The resultant sample was characterized by FT-IR, scanning electron microscopy (SEM), XRD, lipophilic degree (LD) and sedimentation test. The FT-IR results indicated that a covalent bond was formed by chemical reaction between the hydroxyl groups on the surface of Fe₃O₄ nanoparticles and carboxyl groups of stearic acid, which changed the polarity of Fe₃O₄ nanoparticles. The dispersion of Fe₃O₄ in organic solvent was greatly improved. Effects of reaction time, reaction temperature and concentration of stearic acid on particle surface modification were investigated. In addition, Fe₃O₄/polystyrene (PS) nanocomposite was synthesized by adding surface modified Fe₃O₄ magnetic nanoparticles into styrene monomer, followed by the radical polymerization. The obtained nanocomposite was tested by thermogravimetry (TG), differential scanning calorimetry (DSC) and XRD. Results revealed that the thermal stability of PS was not significantly changed after adding Fe₃O₄ nanoparticles. The Fe₃O₄ magnetic fluid was characterized using UV–vis spectrophotometer, Gouy magnetic balance and laser particle-size analyzer. The testing results showed that the magnetic fluid had excellent stability, and had susceptibility of 4.46×10⁻⁸ and saturated magnetization of 6.56 emu/g. In addition, the mean size d (0.99) of magnetic Fe₃O₄ nanoparticles in the fluid was 36.19 nm.     

Determination of cyclosporin A in the serum of kidney transplant patients by rapid-flow fractionation and normal-phase high-performance liquid chromatography

High-performance liquid chromatography was used to determine cyclosporin A (CsA) concentrations in the serum of kidney transplant patients by rapid-flow fractionation (RFF) followed by silica gel normal-phase high-performance liquid chromatography (HPLC). The extraction of CsA from serum was achieved by RFF using a short diatomaceous earth column eluted with diethyl ether-n-hexane (50:50, v/v). The recovery was more than 80% at concentrations of 50-150 micrograms/l. The concentration of this compound was determined by HPLC using a conventional silica gel column with 3.3 M ammonia solution-ethanol-n-hexane (0.31:10.69:89, v/v) as eluent. Concentration calibration was made on the basis of the peak-height ratio of CsA to CsD as the internal standard. The coefficient of variation of this assay was less than 6.5% and the results were used for the therapeutic drug monitoring of CsA administered to kidney transplant patients. Measurements of the CsA concentrations in 160 serum specimens were also made by conventional radioimmunoassay (RIA) using commercial kits. The data obtained by RIA were on average 2.5 times those obtained by HPLC. Higher values in RIA were observed characteristically with patients with severe disfunction resulting from CsA hepatotoxicity. From the results, it appeared that HPLC rather than RIA provides more precise and reliable values for the concentration of this drug.     

Preparation and electrical characterization of (PVC + KBrO3) polymer electrolytes for solid state battery applications

This paper presents results of studies on dc electrical conductivity and transference number measurements on potassium bromate (KBrO₃) complexed polyvinyl chloride (PVC) films prepared by solution cast technique. Temperature dependence of dc electrical conductivity and transference number data indicated the dominance of ion type charge transport in these specimens. The magnitude of conductivity increased with increase in concentration of the salt and temperature. Using this (PVC + KBrO₃) electrolyte, solid-state electrochemical cells were fabricated, and their discharge profiles were studied under a constant load of 100 kΩ. Several cell profiles such as open circuit voltage, short circuit current, power density, and energy density associated with these cells were evaluated and were reported. The features of complexation of the electrolytes were studied by X-ray diffraction and Fourier transform infrared spectroscopy. Paper presented at the Third International Conference on Ionic Devices (ICID 2006), Chennai, Tamilnadu, India, Dec. 7–9, 2006     

Effect of the electric field on “incommensurate-commensurate” magnetic phase transitions in BiFeO3-type multiferroics

The specific features of the “incommensurate-commensurate” phase transitions induced by a magnetic field in multiferroics (materials with coexisting magnetic and electric ordering) are considered. These materials are ferroelectromagnets, for example, bismuth ferrite BiFeO₃ and BiFeO₃-based compounds, which have spatially modulated spin structures. It is shown that the interaction between the electric and magnetic subsystems of the multiferroic material can lead to an electric-field-induced shift of the critical magnetic field corresponding to the transition from a spatially modulated state to a homogeneous antiferromagnetic state. According to the theoretical estimates obtained for material parameters characteristic of the bismuth ferrite, this shift is of the order of 0.5 T in an electric field of 50 kV/cm. The phase diagrams are constructed in the “electric field-magnetic field” coordinates. The results of calculations performed in the harmonic incommensurate structure approximation are compared with the exact soliton solution.     

Synthesis of thiazolo[5,4-b]pyridine-2-carboxamides

A convenient procedure was developed for preparation of thiazolo[5,4-b]pyridine-2-carboxamides by oxidation of monothiooxamides synthesized from 3-aminopyridine.     

Structuring of polyacrylonitrile solutions

Mechanisms of orientation for the solutions of polyacrylonitrile synthesized under conditions of radical and anionic polymerization were studied. The effect of the fractal-matrix structuring agent developed by the AIRES foundation on the correlation parameters of the solution density and average squared fluctuation polarizability, which can be used to determine how the supramolecular structure changes by “self-orientation” and “induced orientation” mechanisms, was analyzed.