AN INTEGRATED CALCIUM-FLUORIDE CRYSTAL IR THIN-LAYER CELL AND ITS APPLICATION TO IDENTIFICATION OF ELECTROCHEMICAL REDUCTION PRODUCT OF BILIRUBIN

An integrated CaF2 crystal optically transparent infrared (ir) thin-layer cell was designed and constructed without using any soluble adhesive materials. It is suitable for both aqueous and nonaqueous systems, and can be used not only in ir but also in uv-vis studies. Excellent electrochemical and spectroelectrochemical responses were obtained in evaluating this cell by cyclic voltammetry and steady-state potential step measurements for both ir and uv-vis spectrolectrochemistry with ferri/ferrocyanide in aqueous solution, and with ferrocene/ferrocenium in organic solvent as the testing species, respectively. The newly designed ir cell was applied to investigate the electrochemical reduction process of bilirubin in situ, which provided direct information for identifying the structure of the reduction product and proposing the reaction mechanism.

The Photovoltage Properties and the Spectrum Analyses of Nanocrystalline Er2O3

The diffuse reflectance spectra of nanocrystalline Er2O3 were measured in the UV-vis region. It was found that the f -> f transition bands become stronger with the decrease of the size of particles. The tail-band in the range of 300 similar to 550nm was assigned to the O2p -> Er4f transition. Both behavior of light-induced charge transfer and photovoltaic properties of nanocrystalline Er2O3 were investigated with surface photovoltage spectroscopy (SPS). The SPS shows that two peaks appear at 340nm (p(1)) and 385nm (p(2)). The observed spectral features can be explained in terms of charge transfer and interband transition.

Characterization of 1:12 Phosphomolybdic Anions Doped Polypyrrole (PMo12/PPy) Film Electrode

1:12 phosphomolybdic anion doped polypyrrole film electrode was characterized by in-situ UV-vis spectroelectrochemistry, X-ray photoelectron spectroscopy(XPS), scan electronic microscopy(SEM) and electron spin resonance(ESR) spectroscopy.

Synthesis of NiWO4 nano-particles in low-temperature molten salt medium

Nickel tungstate (NiWO4) nano-particles were successfully synthesized at low temperatures by a molten salt method, and characterized by Xray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet visible spectra techniques (UV-vis), respectively. The effects of calcining temperature and salt quantity on the crystallization and development of NiWO4 crystallites were studied. Experimental results showed that the well-crystallized NiWO4 nano-particles with about 30 nm in diameter could be prepared at 270 degrees C with 6:1 mass ratio of the salt to NiWO4 precursor. XRD analysis confirmed that the product was a pure monoclinic phase of NiWO4 with wolframite structure. UV-vis spectrum revealed that NiWO4 nano-particles had good light absorption properties in both ultraviolet and visible light region. (C) 2009 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Direct synthesis and characterization of titanium-substituted mesoporous molecular sieve SBA-15

Ti-substituted mesoporous SBA-15 (Ti-SBA-15) materials have been synthesized by using a new approach in which the hydrolysis of the silicon precursor (tetramethoxysilane, TMOS) is accelerated by fluoride. These materials were characterized by powder X-ray diffraction patterns (XRD), X-ray fluorescence spectroscopy (Y-RF), N-2 sorption isotherms, diffuse-reflectance UV-visible (UV-vis) and UV-Raman spectroscopy, Si-29 MAS NMR, and the catalytic epoxidation reaction of styrene. Experiments show that Ti-SBA-15 samples of high quality can be obtained under the following conditions: F/Si greater than or equal to 0.03 (molar ratio), pH less than or equal to 1.0, aging temperature less than or equal to 80 degreesC, and Ti/Si less than or equal to 0.01. It was found that the hydrolysis rate of TMOS was remarkably accelerated by fluoride, which was suggested to play the main role in the formation of Ti-SBA-15 materials of high quality. There is no stoichiometric incorporation of Ti, and the Ti contents that are obtained are quite low in the case of the approach that is proposed. The calcined Ti-SBA-15 materials show highly catalytic activity in the epoxidation of styrene.

Pump-dump control and the related transient absorption spectroscopies

We combine theories of optimal pump-dump control and the related transient probe absorption spectroscopy in order to elucidate the relation between these two optical processes and the possibility of experimental realization. In the weak response regime, we identify the globally optimal pair of pump-dump control fields, and further propose a second-order difference detection scheme to monitor the wave packets dynamics that is jointly controlled by both the pump and dump fields. The globally optimal solution serves also as the initial input for the iterative search for the optimal control fields in the strong response regime. We use a model I-2 molecule to demonstrate numerically the pump-dump control and the detection of a highly vibrationally excited wave packet focusing dynamics on the ground X surface in both the weak and strong response regimes. The I2B surface serves as the intermediate to assist the pump-dump control and the optical detection processes. Demonstrated in the strong response regime are the optimal pair of pump-dump molecular-pi pulses that invert nearly total population onto the predefined target region within a half period of vibration motion. (C) 1999 American Institute of Physics. [S0021-9606(99)00115-4].

Direct synthesis of highly ordered Fe-SBA-15 mesoporous materials under weak acidic conditions

Iron-substituted SBA-15 (Fe-SBA-15) materials have been synthesized via a simple direct hydrothermal method under weak acidic conditions. The powder X-ray diffraction (XRD), NZ sorption and transmission electron microscopy (TEM) characterizations show that the resultant materials have well-ordered hexagonal meso-structures. The diffused reflectance UV-vis and UV resonance Raman spectroscopy characterizations show that most of the iron ions exist as isolated framework species for calcined materials when the Fe/Si molar ratios are below 0.01 in the gel. The presence of iron species also has significant salt effects that can greatly improve the ordering of the mesoporous structure. Different iron species including isolated framework iron species, extraframework iron clusters and iron oxides are formed selectively by adjusting the pH values of the synthesis solutions and Fe/Si molar ratios. (c) 2005 Elsevier Inc. All rights reserved.

Post-grafting preparation of large-pore mesoporous materials with localized high content titanium doping

A new post-grafting process, consisting of two steps of substrate preparation and sol - gel post-grafting, has been developed to prepare titanium-doped mesoporous SBA-15 material with a double-layered structure and locally concentrated titanium content at the inner pore surface. With this novel technique, the single phased and originally ordered mesostructures can be well conserved; in the conventional direct synthesis they can be partially damaged when the frameworks are doped with high content heteroatoms. Titanium species exist in an isolated, tetrahedral structure and are localized at the pore surface; this is beneficial to both reactant access and product release. Characterization with XRD, N-2 adsorption/desorption isotherms, HREM/ EDS, ICP, UV - Vis, and the newly developed UV - Raman spectroscopy confirm these results. Preliminary catalytic tests with the selective epoxidation of cyclohexene show good catalytic activity. Among them, sample TiSBA-15-10 with a Si : Ti molar ratio of 10 shows a TON value of 75 and a highest product ( epoxide) yield of 55%.