Effect of solution chemistry and speciation on shelf-life of silica sols and characteristics of deposited mesoporous thin films.

The effects of storage temperature and time on deposition characteristics of molecularly templated silica sols, used in synthesis of mesoporous silica films, were investigated by preparing acid catalysed water-ethanol-TEOS sols with surfactant and analysing by silicon-29 NMR spectroscopy over a period of multiple days, and by producing films after specific storage times corresponding to collection of NMR spectral data, and analysed for thickness and porosity.

1H dynamic nuclear polarization in supercritical ethylene at 1.4 T.

(1)H dynamic nuclear polarization (DNP) has been measured in supercritical ethylene in the pressure range 60-300 bar in an external field of 1.4 T. A single-cell sapphire tube was used as a high-pressure cell, and powdered 1,3-bisdiphenylene-2-phenyl allyl (BDPA) free radicals were added and distributed at the wall of the cell. At all pressures the dominant DNP mechanism was a positive Overhauser enhancement, caused by proton-electron contact interactions at the fluid/solid radical interface. The observed enhancements varied from 12 at 60 bar to 17 at 300 bar. Besides the Overhauser enhancement, small solid state and thermal mixing enhancements also were observed, indicating that part of the ethylene was adsorbed at the radical surface for a prolonged time. The impacts of the experimental conditions on the Overhauser enhancement factors are discussed, and enhancements of at least 40-60 are estimated when the EPR saturation factor and the leakage factor become maximal. These data indicate that DNP-enhanced NMR has the potential of extending the impact of NMR in research areas involving supercritical fluids.

Physical characterization of PBCV virus by sedimentation field flow fractionation.

A virus (PBCV) from the symbiotic Chlorella-like algae of Paramecium bursaria has been characterized by sedimentation field flow fractionation (SdFFF). The method yields effective molecular weight M' (molecular weight X buoyancy factor) with a precision of better than 5% under a variety of experimental conditions. The value for M' is used to calculate true molecular weight values through combination with density values; densities were obtained from outside sources, from ultrasonic densitometry, and from sedimentation coefficients determined independently. The actual molecular weight is also determined through SdFFF analysis of the virus in carriers of different densities. Values for the particle diameter are obtained from SdFFF zone broadening studies. The various SdFFF characterization results are compared with molecular weight, particle size, and density values determined by conventional methods.