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91.
Phase transition of water restrained by curdlan suspension
annealed at a temperature from 20 to 110°C was investigated by differential
scanning calorimetry (DSC). The melting temperature of water restrained by
annealed curdlan discontinuously decreased at around 60°C, while the amount
of bound water calculated from enthalpy of melting increased at 60°C,
regardless of water content. Using a highly sensitive DSC, curdlan suspension
with various concentrations was studied. It was found that an endothermic
transition was observed at ca. 58°C in a wide range of concentrations.
The transition observed at 60°C is thermo-reversible and both temperature
and transition enthalpy are constant even after gel formation. Well equilibrated
suspension at a temperature lower than 60°C formed no gel. 相似文献
92.
Masuda J Maynard DM Nishimura M Ueda T Kowalak JA Markey SP 《Journal of chromatography. A》2005,1063(1-2):57-69
A one- or two-dimensional high performance liquid chromatography system for electrospray ionization mass spectrometers has been developed that is optimized for ion exchange and reversed phase separations. A unique and simple valve configuration permits the use of a variety of non-volatile salts; ammonium sulfate was used in an example of strong cation exchange separations. The system was designed and evaluated for both micro- and nanoflow chromatography. The peptide detection limit was approximately 100 fmol for micro- and 20 fmol for nanoflow, demonstrating the concentration and mass sensitivity improvements expected with nanoelectrospray ionization. The 1D/2D-HPLC MS system is fully automated for routine peptide analyses, compatible with direct injection of proteolytic digests, and exhibits chromatographic reproducibility and sensitivity. Software permits operator selection of either a 1D or 2D configuration with corresponding system parameters as required for individual samples. The hardware elements and resulting performance are described in this paper. 相似文献
93.
Masafumi Kobayashi Tetsuya Inoguchi Takashi Iida Takashi Tanioka Hiroshi Kumase Yasushi Fukai 《Journal of fluorine chemistry》2003,120(2):2838-110
Direct fluorination of 1,3-dioxolan-2-one with elemental fluorine was successfully carried out to provide 4-fluoro-1,3-dioxolan-2-one, which was expected as an additive for lithium ion secondary battery. 4-Fluoro-1,3-dioxolan-2-one was also further fluorinated with elemental fluorine to give three isomers of difluoro derivatives by the same methodology. Another topic is the preparation of trifluoromethanesulfonyl fluoride, an intermediate of lithium battery electrolyte, by the reaction of methanesulfonyl fluoride with elemental fluorine. The use of perfluoro-2-methylpentane as a solvent gave satisfactory selectivity of trifluoromethanesulfonyl fluoride. 相似文献
94.
The cycloaddition reaction of N-ethoxycarbonyl-1H-azepine with 2,5-dimethoxycarbonyl-3,4-diphenylcyclopentadienone gave anti-endo [4+2]π and exo [6+4]π cycloadducts. These structures were fully identified by X-ray crystallographic techniques. Mechanism for their cycloaddition reactions are also discussed. 相似文献
95.
A novel conjugation-elongated bis(ethylenedithio)tetraselenafulvalene (BETS) type donor, 2,5-bis(4,5-ethylenedithio-1,3-diselenol-2-ylidene)-2,3,4,5-tetrahydrothiophene (BEDT-HBDST) and its magnetic and non-magnetic anion salts, (BEDT-HBDST)2MX4 (MX4−=FeCl4−, GaCl4−, FeBr4− and GaBr4−), were prepared. These four salts are isostructural and belong to the space group of P2/c. They showed semiconducting behavior with small activation energies (59-64 meV). The band structures of these salts are quasi one-dimensional and there is a midgap between the upper band and the lower band, since the degree of dimerization is significant in the stacking direction. The MX4− ions are located between the donor columns and near to the ethylenedithio moieties of the donor molecules. The magnetic susceptibilities of the FeCl4− and FeBr4− salts follow the Curie-Weiss law with Curie constants of 4.6 and 4.8 emu K mol−1 (sum of the spins of S=5/2 and S=1/2) and negative Weiss temperatures of θ=−1.2 and −4.9 K, respectively, revealing a weak antiferromagnetic interaction of 3d spins of the FeCl4− and FeBr4− anions. The Fe?Fe (6.66-7.60 Å), Cl?Cl (4.81-4.82 Å) and Br?Br (4.74-4.77 Å) distances in the crystal structures of these salts are significantly long. Therefore, the direct magnetic interaction between the 3d spins of the nearest neighboring Fe3+ ions appears to be not readily accessible. 相似文献
96.
97.
98.
99.
Hirokazu Morisawa Takashi Utagawa Takeshi Miyoshi Fumihiro Yoshinaga Akihiro Yamazaki Koji Mitsugi 《Tetrahedron letters》1980,21(5):479-482
An enzymatic transarabinosylation between 2-chlorohypoxanthine and 1-β--arabinofuranosyluracil gave 9-β--arabinofuranosyl-2-chlorohypoxanthine which was chemically converted to 9-β--arabinofuranosylguanine and its derivatives. 相似文献
100.
Takashi Kamimura Tsukio Masegi Mitsuo Sekine Tsujiaki Hata 《Tetrahedron letters》1984,25(38):4241-4244
Diisopropylethylamine was effective as a base for acylation of 2′,3′,5′-tri-O-acetyluridine with various acid chlorides. The 13C NMR spectra of the products and related compounds showed clearly that the acyl groups intoduced to the uracil moiety are attached to the N3-nitrogen. 相似文献