Laser Raman and FTIR studies on Li+ interaction in PVAc-LiClO4 polymer electrolytes

The polymer electrolytes composed of poly(vinyl acetate) (PVAc) with various stoichiometric ratios of lithium perchlorate (LiClO(4)) salt have been prepared by solution casting method. The techniques Fourier transform infra-red (FTIR) and Laser Raman spectroscopy have been used to monitor polymer-salt complex formation, ion-ion and ion-polymer interactions as a function of salt concentration. Significant changes in both Laser Raman and FTIR spectra are observed which reveals an interaction between ester oxygens with lithium cation coordination. These results strongly suggest the interaction of lithium cation and network polymer chains. When the salt content is increased, the intensity of the internal Raman modes of the ClO(4)(-) increases. The ClO(4)(-) stretching mode observed at 934 cm(-1) in Laser Raman shows some additional shoulder peaks with increase in salt concentration. This reveals the presence of free anions, ion contact pairs and higher order ionic clusters. From the FTIR and Laser Raman results the transport mechanism of ions in PVAc:LiClO(4) polymer electrolytes has been discussed.     

Facile isolation ofEndo-pectate lyase fromErwinia carotovora based on electrostatic interaction

Endo-pectate lyase (PATE) from Erwinia carotovora was selectively cosedimented with extracellularly produced lipopolysaccharide-lipid complex (LPSLC) through dialysis of the cell free culture broth. The selective isolation of PATE was confirmed by sodium dodecyl sulfate polyacrylamide gel electrophoresis. The cosedimentation of the PATE with LPSLC was initiated by decreasing conductivity of the solution and terminated at approx 1 m siemens (mScm-1). As much as 62% of PATE activity in the culture broth was removed by precipitation. PATE was isolated from the precipitate by gel chromatography. The cosedimentation of PATE with LPSLC was remarkably affected by pH or ionic strength. The addition of polycationic peptide polymyxin B sulfate or a metal chloride affected the interaction. The cosedimentation was diminished by acetylation of the free amino groups of PATE. From these results, it was confirmed that the cosedimentation was induced by electrostatic interaction.     

Structural and impedance analysis of LiBiP2O7

A new material LiBiP₂O₇ was prepared by solid-state reaction method. The XRD analysis confirms the formation of the sample. The Raman analysis indicates the presence of characteristic bands for a (P₂O₇)⁴⁻ group in the sample. The electrical characterization was carried out using the impedance spectroscopy method in the frequency range of 1 KHz–5 MHz. The bulk conductivity of the material was extracted from the impedance analysis and was found to be in the order of 10⁻⁷ Ω ⁻¹ cm⁻¹ at 473 K. The activation energy was calculated from the Arrhenius plot and was found to be 0.37 eV. The modulus peak maximum shifts to higher frequencies with an increase in temperature and the broad nature of the peaks indicates the non-debye nature of the material. The high value for the activation energy calculated from the conductance spectrum indicates that some energy has been utilized in the creation of charge carriers.     

Pseudo-conformal quaternionic CR structure on (4n + 3)-dimensional manifolds

We study an integrable, nondegenerate codimension 3-subbundle ${\mathcal{D}}We study an integrable, nondegenerate codimension 3-subbundle on a (4n + 3)-manifold M whose fiber supports the structure of 4n-dimensional quaternionic vector space. It is thought of as a generalization of quaternionic CR structure. We single out an -valued 1-form ω locally on a neighborhood U such that and construct the curvature invariant on (M, ω) whose vanishing gives a uniformization to flat quaternionic CR geometry. The invariant obtained on M has the same formula as that of pseudo-quaternionic K?hler 4n-manifolds. From this viewpoint, we exhibit a quaternionic analogue of Chern-Moser’s CR structure. The authors are grateful to ESI for financial support and hospitality during the preparation of this work. The first author acknowledge the support by Grant FWF Project P17108-N04 (Vienna) and Grant N MSM 0021622409 of the Ministry of Education, Youth and Sports (Brno).     

Magnetic property of pyrolytic carbon prepared on diamond powder in applied magnetic field

We have prepared pyrolytic carbon samples from triethylamine on diamond powder in applied magnetic field of 6 T and investigated their magnetic properties. A ferromagnetic sample was obtained from the pyrolysis products even at room temperature, with spontaneous magnetization of 6.4 A m²/kg at 300 K, which is twice as large as that of the sample prepared without diamond powder. Therefore, the diamond powder seems to promote the formation of a three-dimensional ferromagnetic structure in pyrolytic carbon.     

Uronic acid determination by high performance liquid chromatography with postcolumn fluorescence derivatization

To develop a fluorimetric high performance liquid chromatography (HPLC) technique for uronic acid microanalysis, a saline mobile phase and the postcolumn fluorimetric determination were combined. The detection limits of D-glucuronic, D-galacturonic and D-mannuronic acids were 7.19, 23.88 and 7.08 pmol, respectively. The proposed method was successfully applied to uronic acid microanalysis in a polysaccharide hydrolysate and a drink.     

Estimation of inter-atomic force constants and phonon dispersion using correlation effects among thermal displacement of atoms in Ge

Neutron diffraction measurements have been performed on powder Ge at 6, 150 and 300 K. Oscillatory diffuse scattering intensity is clearly observed at 150 and 300 K. The diffuse scattering theory including correlation effects among thermal displacements of atoms is applied to background function in the Rietveld analysis. The inter-atomic distance and temperature dependence of the values of correlation effects are discussed. The force constants among the first, second and third nearest neighboring atoms in Ge are obtained from the values of correlation effects and Debye-Waller temperature parameters. A phonon dispersion spectrum in Λ [111] direction for Ge crystal has also been calculated at 80 K using inter-atomic force constants and the crystal structure.     

Thermal square planar-to-octahedral transformation of nickel(II) complexes containing butanediamines in a solid phase

Thermal reactions of the nickel(II) complexes, [Ni(m-bn or i-bn)₂]X₂ and [Ni(H₂O)₂(dl-bn)₂]X₂·n H₂O, where m-bn, i-bn, and dl-bn are meso-2,3-butanediamine, 2-methyl-1,2-propanediamine, and dl-2,3-butanediamine, respectively, X is Cl^?, Br^?, I^?, NO^?₃, or ClO^?₄, and n is 2 for bromide, and 0 for the others, were investigated in a solid phase before and after heating using thermal analyses (TG and DSC) and spectral and magnetic measurements. In the case of the chloride and bromide, the square planar bis(dl-bn) complexes obtained by dehydration of the respective diaqua complexes were transformed to the octahedral diacido bis(dl-bn) complexes upon further heating. The same structural transformation was observed in the thermal reactions of [Ni(m-bn)₂](NO₃)₂ and [Ni(i-bn)₂]Cl₂. It was summarily recognized that such square planar-to-octahedral transformation was favored in the order dl-bn > i-bn > m-bn complexes in the respective halides, and it was a reversible thermochromism from yellow to blue. The changes in enthalpy of the reactions were endothermic and fell in the range of about 10–20 kJ mole^?1. The possibility of such configurational change seems to be dependent mainly upon the ionic radius of the X anion, the orientation of two C-substituted methyl groups on butanediamines in the formation of the complexes, and the thermal stability of the complexes themselves.     

Simultaneous analysis of monosaccharides and oligosaccharides by high-performance liquid chromatography with postcolumn fluorescence derivatization

To develop a fluorimetric HPLC technique for the simultaneous microanalysis of reducing mono- and oligosaccharides, the technique of linear gradient elution was introduced into the postcolumn fluorimetric detemination system of reducing saccharides with benzamidine. Fluorescence measurement was performed at 288 nm for excitation and 470 nm for emission and an optimization study for this postcolumn fluorescence derivatization carried out. Under optimum conditions, the detection limits of D-glucose and maltohexaose were 1.78 and 2.59 pmol, respectively. The present method was successfully applied to saccharide analysis and should prove useful for automated simultaneous microanalysis of reducing mono- and oligosaccharides in foods.