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541.
542.
Masayoshi Tabata Yoshikazu Sadahiro Takeyuki Sone Kazuaki Yokota Yuichi Ishikawa 《Journal of polymer science. Part A, Polymer chemistry》1998,36(14):2457-2461
Alkylpropiolate having n-hexadecyl moiety in the ester group was stereospecifically polymerized with a [Rh(norbornadiene)Cl]2 complex catalyst in alcohol to give rise to cis-transoid polyacetylenes in high yields. The unusually facile cis to trans isomerization for the polymer was found to be induced when the polymer was warmed to even less than ca. 57°C. Under these conditions ESR spectra bearing hyperfine structures due to the radicals generated by the rotational scission in the cis–π bond were observed. This isomerization induced a large g value shift in the ESR spectra together with an increase of the radical concentration during the isomerization, indicating formation of planar conjugated trans sequences that stabilize mobile unpaired electrons as solitons. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2457–2461, 1998 相似文献
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545.
This article describes a novel idea on preparation of a glass bead for X-ray fluorescence spectrometry, to determine alloyed elements in high-speed steel without any matrix correction. The quantification method using the glass bead is generally effective to reduce secondary X-ray absorption and enhancement (matrix effect) by coexisting elements in a sample. Although the glass bead is normally prepared based on a flux-to-sample ratio, the suggested method mainly controls an absolute amount of the sample in the glass bead to prevent from any interference with the matrix elements. As a result, the alloyed elements, except tungsten, in high-speed steels could be determined with high precision and accuracy, independent of the flux-to-sample ratio. However, the fluorescent X-ray intensity of tungsten Lα line (8.40 keV) was obviously influenced by the sample amount (iron content) in a glass bead; in this case, the Mα line (1.77 keV) could be employed alternatively. 相似文献
546.
Kazuaki Ito Takanori Ohta Yoshihiro Ohba Tyo Sone 《Journal of heterocyclic chemistry》2000,37(1):79-85
Chiral bishomodiazacalix[4]arenes containing amino acid residues were prepared. The 1H and 13C nmr spectra indicated that the macrocycles preferably adopted a cone conformation, which suggested that the cyclophane moiety was in a chiral twisted form. Circular dichroism spectra supported the existence of the chirality of the cyclophane unit, and showed that intramolecular hydrogen bonding plays an important role in the transmission of the chirality from the amino acid residues to the cyclophane moiety. Macrocycles bearing a tyrosine residue have a π‐base cavity large enough to include the ammonium ion, and can serve as a shift reagent for the racemic ammonium ions upon complexation during a 1H nmr analysis. 相似文献
547.
Utilising extremely different vaporisation properties of boron compounds, the determination procedures of volatile boric acid and total boron using tungsten boat furnace (TBF) ICP-MS and TBF-ICP-AES have been investigated. For the determination of volatile boric acid by TBF-ICP-MS, tetramethylammonium hydroxide (TMAH, Me4NOH) was used as a chemical modifier to retain it during drying and ashing stages. As for the total boron, not only non-volatile inorganic boron such as boron nitride (BN), boron carbide (B4C), etc. but also boric acid (B(OH)3) was decomposed by a furnace-fusion digestion with NaOH to produce sodium salt of boron, a suitable species for the electrothermal vaporisation (ETV) procedure. The proposed method was applied to the analysis of various standard reference materials. The analytical results for various biological and steel samples are described. 相似文献
548.
Oxidation of methyl glycopyranosides with periodic acid in pyridine was studied by analysis of the reaction products by the dithioacetal method. Both C2—C3 and C3—C4 bonds were cleaved yielding three types of dialdehydes;secondary attack of these dialdehydes by periodic acid did not occur. Oxidation in aqueous pyridine proceeded in normal Malapradian fashion, but more slowly than for oxidation in water. Molar proportions of aldehydes were theoretical, when methyl glycosides were oxidized with periodic acid in a 1:1 () mixture of pyridine and water. The structures of carbohydrate moieties in a few saponins and glycolipids were confirmed by analysis of the oxidation products obtained under similar conditions. 相似文献
549.
Hiroko Seki Yoshihisa Sei Kazuaki Shikii Sakurako Shimotakahara Hiroaki Utsumi Kentaro Yamaguchi Mitsuru Tashiro 《Analytical sciences》2004,20(10):1467-1470
A difference diffusion-based NMR technique and cold-spray ionization mass spectrometry were employed as a solution-based approach for identifying a ligand binding with a protein receptor. The difference diffusion-based NMR technique, called difference NOE-pumping, can directly detect the ligand interacting with a protein receptor. This technique uses a simple pulse sequence and the diffusion filter can easily be optimized. The cold-spray ionization mass spectrometry (CSI-MS), a variant of electrospray ionization mass spectrometry (ESI-MS) operating at low temperature, has been applied to detect the ligand-receptor complex. The efficiency of these techniques for identifying binding ligands is demonstrated with the human serum albumin (HSA)-drug system. 相似文献
550.