Solid dispersion particles of tolbutamide prepared with fine silica particles by the spray-drying method

Solid dispersion particles of tolbutamide (TBM) were prepared by formulating nonporous (Aerosil 200 (hydrophilic), Aerosil R972 (hydrophobic)) or porous (Sylysia 350 (hydrophilic), Sylophobic 200 (hydrophobic)) silica as a carrier and applying the spray-drying (SD) or evaporation (Eva) method. In the solid dispersion particles prepared by the SD method, TBM existed in a meta-stable form (Form II) irrespective of the type of silica. On the other hand, when the Eva method was used, various crystalline forms of TBM were observed in the solid dispersion particles according to the type of silica. Polymorphs of Forms III and IV were prepared with Aerosil 200 and Aerosil R972, respectively, while crystalline Form II was obtained when either of the forms of porous silica, Sylysia 350 or Sylophobic 200, was formulated. The dissolution property of TBM in the solid dispersion particles prepared with hydrophilic silica was remarkably improved compared with those of the original TBM crystals (Form I) or spray-dried TBM without silica (Form II). In the case of hydrophobic silica, the release rate of TBM from the solid dispersion particles was much slower than that of original TBM. The meta-stable form of TBM in the solid dispersion particles was stable for at least 4 weeks when stored at 60 °C and 0% RH, while the spray-dried TBM without silica (Form II) was gradually converted to the stable form (Form I) under the same storage conditions. Under the humid storage conditions (60 °C, 75% RH), the spray-dried TBM without silica (Form II) immediately converted into the stable form (Form I) within 1 day, while TBM (Form II) in the solid dispersions in a matrix of silica was stable for at least 1 week.     

Anatase Sol Prepared from Peroxotitanium Complex Aqueous Solution Containing Niobium or Vanadium

Niobium- or vanadium-doped anatase sols were prepared by hydrothermal treatment of 0.1 mol/dm³ peroxotitanium complex aqueous solutions dissolving 0–10 mol% niobium or vanadium at 100°C for 8 h. Niobium-doping caused the increase of lattice constants of anatase and the shape change of anatase crystal from spindle-like to cubic-like structure, but no change of the optical absorbance. Vanadium-doping caused the decrease of lattice constant of c -axis, the miniaturization of anatase crystal and the increase of optical absorbance at the wavelength from 350–700 nm.     

SOLVENT EXTRACTION OF ZINC FROM CHLORIDE MEDIA WITH SECONDARY LONG-CHAIN ALKYLAMINE

In the solvent extraction of zinc from chloride media with a secondary long-chain alkylamine, Amberlite LA-2, aggregations of ammonium chloride salt of alkylamine and zinc-complex with alkylamine and distribution equilibrium of zinc were investigated at 30 "C using n-hexane as a diluent. The ammonium chloride salt of alkylamine exists as monomeric, dimeric, trimeric and tetrameric species (BHCl, (BHCl)₂, (BHCl)₃ and (BHCl)₄, respectively). The zinc-complex exists as monomeric and dimeric species ((BH)₂ZnCl₄ and ((BH)₂ZnCl₄)₂, respectively). Zinc is extracted according to the extraction reaction in the lower loading region of zinc to alkylamine and according to the extraction reaction in the higher loading region.     

Regio‐ and Stereochemical Controlled Koenigs–Knorr‐Type Monoglycosylation of Secondary Hydroxy Groups in Carbohydrates Utilizing the High Site Recognition Ability of Organotin Catalysts

The catalytic regio‐ and stereoselective monoglycosylation of carbohydrates using organotin catalysts is demonstrated. The one‐step reaction affords various oligosaccharides linked at the secondary hydroxy group in high chemical yield and good regio‐ and stereoselectivities. The regioselectivity of the glycosylation is shown to depend on the spatial arrangement of the hydroxy groups in the carbohydrates.

     

Polymer electrolyte membrane with nanomatrix channel prepared by sulfonation of natural rubber grafted with polystyrene

High‐proton‐conductive polymer electrolyte with a nanomatrix channel was prepared by graft copolymerization of styrene onto deproteinized natural rubber followed by sulfonation with chlorosulfonic acid. First, natural rubber latex was purified with urea in the presence of surfactant to remove almost all proteins present in the rubber. Second, graft copolymerization of styrene onto deproteinized natural rubber was carried out with tert‐butyl hydroperoxide/tetraethylenepentamine as an initiator at 30°C in latex stage. The graft‐copolymerized natural rubber (DPNR‐graft‐PS) was sulfonated with chlorosulfonic acid in chloroform solution at an ambient temperature. The resulting sulfonated DPNR‐graft‐PS was characterized by FTIR spectroscopy, solid state ¹³C CP/MAS NMR spectroscopy, elemental analysis, and transmission electron microscopy. High proton conductivity of about 0.1 S/cm, less water uptake of 24 wt % and comparatively good stress at break of 9 MPa were accomplished at suitable contents of styrene units and sulfur, i.e., 32 wt % and 75 mol %, respectively. The high proton conductivity, excellent stability, and good mechanical properties were associated with not only the formation of the nanomatrix channel but also a specific concentration of sulfuric acid group. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011.     

Intrinsic Elastic, Dielectric, and Piezoelectric Losses in Lead Zirconate Titanate Ceramics Determined by an Immittance-Fitting Method

The material coefficients of "soft" and "hard" lead zirconate titanate (PZT) ceramics were determined as complex values by the nonlinear least-squares-fitting of immittance data measured for length-extensional bar resonators. The piezoelectric d -constant should be a complex value to obtain a best fitting between observed and calculated results. Because the elastic, dielectric, and piezoelectric losses determined in this process were not "intrinsic" losses, a calculation process to evaluate the "intrinsic" losses was proposed. It was confirmed that the intrinsic losses were smaller than the corresponding extrinsic losses. The intrinsic piezoelectric loss existed in both soft and hard PZTs; ∼50% of the loss of piezoelectric d -constant was derived from the elastic and dielectric losses. The most notable difference between the soft and hard PZTs was observed in their elastic losses.     

Direct Electroplating of Lithium Cobalt Oxide Film on Platinum Substrate in 100°–200°C Aqueous Solution

Well crystallized, shape-formed, and electrochemically active lithium cobalt oxide (LiCoO₂) films are electroplated directly on an electron-conducting substrate in an aqueous solution using a soft solution processing that is economical, consumes less energy consuming, and is environmentally friendly. Although LiCoO₂ films are easily and economically prepared without any post-synthesis heat treatment, the estimated film properties show a possibility of using the deposited films as a cathode film for lithium rechargeable microbatteries. In addition, the soft solution processing reveals that an exact understanding of chemical reactions and the proper combination of the chemical reactions can create an advanced synthetic procedure.     

Application of tritium radioluminography to the detection of hydrogen diffusion in Ti-Cr alloy

Tritium radioluminography has been applied to determine the hydrogen (H) diffusion coefficients in Ti₅₀Cr₅₀ and Ti₄₀Cr₆₀ alloys, both with two-phase structures of a body-centered cubic (bcc) phase and a Laves phase. Using radioluminography, H distributions in those phases have been observed, and H penetration profiles have been measured. The tritium diffusion coefficients in the Ti₅₀Cr₅₀ and Ti₄₀Cr₆₀ alloys have been successfully determined by analyzing the tritium penetration profiles to be 3.3±0.3 × 10^?12 and 1.4±0.1×10^?12 m²/s, respectively. These values suggest that the H diffusion in the Laves phase is slower than that in the bcc phase. It is also suggested that H diffuses by short-circuiting diffusion through the interface between the bcc phase and the Laves phase.