SOLID-STATE C-13 NMR-STUDIES ON THE CONDENSATION AND SULFONATION OF FURFURYL ALCOHOL AND TRIS (2-HYDROXYETHYL) ISOCYANURATE

The condensation and sulfonation of furfuryl alcohol (FA) and FA with tris (2-hydroxyethyl) isocyanurate (THEIC) and the crosslinking product structures were studied by means of solid-state C-13 NMR. The reaction of formalin with FA linear oligomer terminated by 2-methyl furan took place in the presence of the phase transfer catalyst (C4H9)4N+I-. The reaction of the terminated oligomer with a large amount of sulfuric acid as well as the former reaction was examined. The effects of some main reaction conditions on the crosslinking condensation and sulfonation were also discussed.

THE CRYSTALLIZATION BEHAVIOUR OF BLOCK COPOLYMER/HOMOPOLYMER BLENDS I. INFLUENCE OF NONSPHERICAL MICELLE ON CRYSTALLIZATION BEHAVIOUR IN DILUTE SOLID SOLUTIONS

The effect of micelle on crystallization behaviour of dilute poly(methyl methacrylate-b-tetrahydrofuran) diblock copolymer/tetrahydrofuran homopolymer, dilute poly (ethylene-b-styrene-b-ethylene) triblock copolymer/ethylene homopolymer solutions has been studied. The results show that with the structural teansitions from spherical to nonspherical micelle in the blends, great changes in the nucleation and spherulite morphologies take place.

Photocatalytic degradation of CI Acid Blue 80 in aqueous suspensions of titanium dioxide under sunlight

The dye C.I. Acid Blue 80 (AB80) was easily degraded by TiO2-P25 assisted photocatalysis in aqueous dispersion under irradiation of sunlight. The optimal reaction conditions were [TiO2] = 2.0 g/L, pH = 10, [H2O2] = 5 mmol/L. The photocatalytic reaction followed pseudo-first order kinetics. The adsorption of AB80 onto TiO2 was in accord with Langmuir equation.

Analysis of urinary 8-hydroxydeoxyguanosine by capillary electrophoresis and solid-phase extraction

Urinary 8-hydroxydeoxyguanosine (80HdG) has been considered as an excellent marker of individuals at high risk of developing cancer. Until now, urinary 80HdG has largely been measured by high-performance liquid chromatography with electrochemical detection. A new method for the analysis of urinary 80HdG by high-performance capillary electrophoresis has been developed and optimized in our laboratory. A single step solid-phase extraction procedure was optimized and used for extracting 80HdG from human urine. Separations were performed in an uncoated silica capillary (50 cm x 50 tm i.d.) using a P/ACE MDQ system with UV detection. The separation of 80HdG from interfering urinary matrix components is optimized with regard to pH, applied voltage, pressure injection time and concentration of SDS in running buffer. The detection limit of this method is 0.4 mug/ml, the linear range is 0.8-500 mug/ml, the correlation coefficients levels is better than 0.999. The developed method is simple, fast and good reproducibility, furthermore, it requires a very small injection volumes and low costs of analysis, which makes it possible to provide a new noninvasive assay for an indirect measurement of oxidative DNA damage.

Fabrication and testing of a doped lanthanum gallate electrolyte thin-film solid oxide fuel cell

A supported lanthanum gallate (LSGM) electrolyte thin-film solid oxide fuel cell with Ni-YSZ cermet anode and strontium-doped lanthanum manganite (LSM)-yttria stabilized zirconia (YSZ) composite cathode was, for the first time, fabricated and tested. The cell was prepared by an unconventional approach, in which an LSGM thin film (about 15 mum thick) was first deposited on a porous substrate such as a porous YSZ disk by a wet process and sintered at a high temperature (above 1400degrees C). NiO was then incorporated into the porous substrate by a carefully controlled impregnation process and fired at a much lower temperature. In this way, the severe reaction between LSGM and NiO at a high temperature, which is required for the full densification of LSGM film, can be avoided. A strontium-doped LaMnO3 (LSM)-YSZ composite cathode was screen printed on the surface of the LSGM film and then fired at 1250degrees C. The electrolyte resistances of the SOFC single cells fabricated by this approach are much lower compared to those of thick LSGM film supported cells. A maximum output power density of over 0.85 W/cm(2) at 800degreesC with H-2 as fuel and air as oxidant for a fabricated cell was achieved. (C) 2002 The Electrochemical Society.

In situ solid state NMR observation of the methanol-to-hydrocarbons (MTH) process over nanosized and microsized HZSM-5 zeolites

The formation of surface alkoxy species on nanosized HZSM-5 and microsized HZSM-5, after exposure to methanol and subsequent conversion to olefins, has been investigated by in situ solid state NMR. Compared to microsized HZSM-5 zeolite, the nanosized HZSM-5 zeolite was found to exhibit a higher affinity for trapping methanol species. Activation of the adsorbed methanol species resulted in the formation of various surface alkoxy species with different rigid characters, including the carboxylate-like surface species, as evidenced by deconvolution of the related spectra. The present results support the existence of the so-called carbon-pool in the conversion of methanol, which serves as the reaction precursor not only for the coupling of the species to form olefins, but also for uncontrolled polymerization to give coke on the surface. The nanosized HZSM-5 shows a distinct resistance to the formation of carbonaceous deposits on the surface.

A high-resolution solid-state NMR study on nano-structured HZSM-5 zeolite

Variations in the structure and acidity properties of HZSM-5 zeolites with reduction in crystal sizes down to nanoscale (less than 100 nm) have been investigated by XRD, TEM and solid-state NMR with a system capable of in situ sample pretreatment. As evidenced by a combination of Al-27 MAS NMR, Si-29 MAS, CP/MAS NMR and H-1 MAS NMR techniques, the downsize of the zeolite crystal leads to an obvious line broadening of the Al-27, Si-29 MAS NMR spectrum, an increasing of the silanol concentration on the external surface, and a pronounced alteration of the acidity distribution between the external and internal surfaces of the zeolite. In a HZSM-5 zeolite with an average size at about 70 nm, the nonacidic hydroxyl groups (silanols) are about 14% with respect to the total amount of Si, while only 4% of such hydroxyl groups exist in the same kind of zeolite at 1000 nm crystal size. The result of H-1 MAS NMR obtained using Fluorinert(R) FC-43 (perfluorotributyl amine) as a probe molecule demonstrates that most of the silanols are located on the external surface of the zeolite. Moreover, the concentration of Bronsted acid sites on the external surface of the nano-structured zeolite appears to be distinctly higher than that of the microsized zeolite.

Electrochemical performance of mixed ionic-electronic conducting oxides as anodes for solid oxide fuel cell

Mixed ionic-electronic conducting (MIEC) oxides, SrFeCo0.5Ox, SrCo0.8Fe0.2O3-delta and La0.6Sr0.4Fe0.8Co0.2O3-delta have been synthesized and prepared on yttria-stabilized zirconia as anodes for solid oxide fuel cells. Power output measurements show that the anodes composed of such kinds of oxides exhibit modest electrochemical activities to both H-2 and CH4 fuels, giving maximum power densities of around 0.1 W/cm(2) at 950 degrees C. Polarization and AC impedance measurements found that large activation overpotentials and ohmic resistance drops were the main causes for the relative inferior performance to the Ni-YSZ anode. While interlayered with an Ni-YSZ anode, a significant improvement in the electrochemical performance was observed. in particular, for the SrFeCo0.5Ox oxide interlayered Ni-YSZ anode, the maximum power output reaches 0.25 W/cm2 on CH,, exceeding those of both SrFeCo0.5Ox and the Ni-YSZ, as anodes alone. A synergetic effect of SrFeCo0.5Ox and the Ni-YSZ has been observed. Future work is needed to examine the long-term stability of MIEC oxide electrodes under a very reducing environment. (C) 1999 Elsevier Science B.V. All rights reserved.