An Application of Silica‐Based Monolithic Membrane Emulsification Technique for Easy and Efficient Preparation of Uniformly Sized Polymer Particles

Summary: Uniformly sized polymer particles were prepared by an emulsification and polymerization technique utilizing a silica monolithic membrane, namely the “silica monolithic membrane emulsification technique”. In this paper, we utilized silica monolithic membrane as a device for the preparation of uniformly sized polymer particles. A mixture of monomers, diluents and oil‐soluble initiator was emulsified into a continuous medium through the silica monolithic membrane and polymerized. The particles obtained had a higher size uniformity than that of particles prepared by previously reported membrane emulsification techniques, such as the Shirasu Porous Glass (SPG) emulsification technique. Through the silica monolithic membrane emulsification technique, we could prepare particles having availability as a possible packing material for solid‐phase extraction (SPE) and high performance liquid chromatography (HPLC).

SEM photograph of silica particles prepared through capillary plate membrane.     

Experimental confirmation of the isotopic volume effect in superconducting molybdenum by means of energy-dispersive x-ray diffration at low temperatures

Differences in the lattice constants of Mo-100 and Mo-92 have been measured by x-ray diffraction, in order to search directly for the volume effect of isotopes in a superconductor. No significant difference in the lattice constanta(Mo-100)–a(Mo-92) could be detected at 290 K, while the differences –0.0014±0.0008 and –0.0029±0.0009 Å were detected at 85.3 and 4.31 K, respectively. These values, and their temperature dependence, are considered to be theoretically reasonable. The exponent in the isotope effect defined by T_cM^- is represented thermodynamically by =–( lnT _c / lnM)–( lnT _c / lnV)(d lnV/d lnM). From the results, d lnV/d lnM is found to be –0.033±0.009 at 4.31 K. Then, the second term representing the isotopic volume effect is estimated to be about 0.09, with lnT _c / lnV2.81. The observed value of is 0.33, so that the contribution of the second term, 0.09, is 27% of the value of . It becomes quite clear that the isotopic volume effect in superconducting Mo should not be neglected.     

Multinomial Bayesian learning for modeling classical and nonclassical receptive field properties

We study the interplay of Bayesian inference and natural image learning in a hierarchical vision system, in relation to the response properties of early visual cortex. We particularly focus on a Bayesian network with multinomial variables that can represent discrete feature spaces similar to hypercolumns combining minicolumns, enforce sparsity of activation to learn efficient representations, and explain divisive normalization. We demonstrate that maximal-likelihood learning using sampling-based Bayesian inference gives rise to classical receptive field properties similar to V1 simple cells and V2 cells, while inference performed on the trained network yields nonclassical context-dependent response properties such as cross-orientation suppression and filling in. Comparison with known physiological properties reveals some qualitative and quantitative similarities.     

Fabrication of Low-Porosity Indium Tin Oxide Ceramics in Air from Hydrothermally Prepared Powder

Compositionally homogeneous indium tin oxide (ITO) ceramics with low porosity were obtained successfully by sintering hydrothermally prepared powders. The fabrication technique began with the preparation of microcrystalline, homogeneously tin-doped (5 wt%) indium oxyhydroxide powder, under hydrothermal conditions. Low-temperature (∼500°C) calcination of the hydrothermally derived powder led to the formation of a substitutional-vacancy-type solid solution of In₂Sn_{1− x} O_{5− y} , and further heating of this phase at temperatures of >1000°C resulted in the formation of the tin-doped indium oxide phase, which had the C -type rare-earth-oxide structure. The sintering of uniformly packed, calcined powder compacts at 1450°C for 3 h in air resulted in low-porosity (∼0.7%) ITO ceramics.     

Performance of a monolithic silica column in a capillary under pressure-driven and electrodriven conditions

A continuous macroporous silica gel network was prepared in a fused-silica capillary and evaluated in reversed-phase liquid chromatography. Under pressure-driven conditions, the monolithic silica column derivatized to C18 phase (100 microns in diameter, 25 cm in length, silica skeleton size of approximately 2.2 microns) produced plate heights of about 23 and 81 microns at 0.5 mm/s with a pressure drop of 0.4 kg/cm2, and at 4.0 mm/s with 3.6 kg/cm2, respectively, in 90% acetonitrile for hexylbenzene with a k value of 0.7. The separation impedance, E, calculated for the present monolithic silica column was much smaller at a low flow rate than those for particle-packed columns, although higher E values were obtained at a higher flow rate. Considerable dependence of column efficiency on the linear velocity of the mobile phase was observed despite the small size of the silica skeletons. A major source of band broadening in the HPLC mode was found in the A term of the van Deemter equation. The performance of the continuous silica capillary column in the electrodriven mode was much better than that in the pressure-driven mode. Plate heights of 7-8 microns were obtained for alkylbenzenes at 0.7-1.3 mm/s, although the electroosmotic flow was slow. In HPLC and CEC mode, the dependency of plate height on k values of the solutes was observed as seen in open tube chromatography presumably due to the contribution of the large through-pores. Since monolithic silica capillary columns can provide high permeability, the pressure-driven operation at a very low pressure can afford a separation speed similar to CEC at a high electric field.     

Mutation analysis of the WT1 gene in myelodysplastic syndromes

Infectious mononucleosis due to Epstein-Barr virus (EBV) is almost always a self-limited disease, most commonly seen in young adults. Hepatitis is a well-recognized complication of EBV infection that usually resolves spontaneously. Jaundice occasionally results from the unusual complication of autoimmune haemolytic anaemia rather than hepatitis. We report a 60-year-old man with severe cholestatic jaundice whose history, liver histology and laboratory findings suggested EBV infection. He also developed significant jaundice related to his hepatitis, but not to autoimmune haemolysis, a situation that led to diagnostic delay. Costly diagnostic laboratory tests and invasive procedures were performed to rule out a malignant extrahepatic biliary obstruction. Physicians need to be aware of this complication and EBV infection should be included in the differential diagnosis of cholestatic jaundice in the elderly.     

Hydrothermal crystal growth of perovskite-type fluorides

Single crystals of perovskite-type fluorides were grown from potassium fluoride and di-valent metal chloride solutions by a hydrothermal method under a temperature gradient, at maximum temperature 600° C and pressure 98 MPa. Single-crystal cubes of KMnF₃, KFeF₃, KCoF₃ and KZnF₃, of cube edge sizes ranging from 0.2 to 2.0 mm, were grown. Crystals of KNiF₃ grew in rectangular prisms and those of KCdF₃ in anhedral form. Single crystals of KCuF₃ were grown in pure water from co-precipitated KCuF₃ powder. KMgF₃ crystals were not grown by this method.     

Simple and comprehensive two-dimensional reversed-phase HPLC using monolithic silica columns

Simple and comprehensive two-dimensional (2D)-HPLC was studied in a reversed-phase mode using monolithic silica columns for second-dimension (2nd-D) separation. Every fraction from the first column, 15 cm long (4.6-mm i.d.), packed with fluoroalkylsilyl-bonded (FR) silica particles, was subjected to the separation in the 2nd-D using one or two octadecylsilylated (C(18)) monolithic silica columns (4.6-mm i.d., 3 cm). Monolithic silica columns in the 2nd-D were eluted at a flow rate of up to 10 mL/min with separation time of 30 s that meets the fractionation every 15-30 s at the first dimension (1st-D) operated at a flow rate of 0.4-0.8 mL/min. Three cases were studied. (1) In the simplest scheme of 2D-HPLC, effluent of the 1st-D was directly loaded into an injector loop of 2nd-D HPLC for 28 s, and 2 s was allowed for injection. (2) Two six-port valves each having a sample loop were used to hold the effluent of the 1st-D alternately for 30 s for one 2nd-D column to effect comprehensive 2D-HPLC without the loss of 1st-D effluent. (3) Two monolithic silica columns were used for 2nd-D by using a switching valve and two sets of 2nd-D chromatographs separating each fraction of the 1st-D effluent with the two 2nd-D columns alternately. In this case, two columns of the same stationary phase (C(18)) or different phases, C(18) and (pentabromobenzyloxy)propylsilyl-bonded (PBB), could be employed at the 2nd-D, although the latter needed two complementary runs. The systems produced peak capacity of approximately 1000 in approximately 60 min in cases 1 and 2 and in approximately 30 min in case 3. The three stationary phases, FR, C(18), and PBB, showed widely different selectivity from each other, making 2D separations possible. The simple and comprehensive 2D-HPLC utilizes the stability and high efficiency at high linear velocities of monolithic silica columns.