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91.
A redox species was extracted from water (50 x 10(-6) dm3) into a single micro-oil-droplet (30 x 10(-12) dm3) in contact with a microelectrode using microcapillary injection and manipulation techniques. Further, an in situ microanalysis of the solute in a single oil droplet was demonstrated by differential pulse voltammetry. The redox species of 10(-16) mol concentrated in the droplet could be quantitatively analyzed independently of the distribution coefficient of the solute between the oil and water phases. The potential of this technique was considered in terms of the preconcentration and separation as well as a microanalysis and an ultratrace analysis. 相似文献
92.
93.
Y. Furukawa H. Terao H. Ishihara T. M. Gesing J.-C. Buhl 《Hyperfine Interactions》2004,159(1-4):143-148
The crystal structure of [C(NH2)3]2HgBr4 has been determined at room temperature: monoclinic, space group C2/c, with a = 10.035(2), b = 11.164(2), c = 13.358(3) Å, β = 111.67(3)°, and Z = 4. The crystal consists of planar [C(NH2)3]+ and distorted tetrahedral [HgBr4]2? ions. The Hg atom is located on a two-fold axis such that two sets of inequivalent Br atoms exist in an [HgBr4]2? ion. In accordance with the crystal structure, two 81Br NQR lines widely separated in frequency were observed between 77 and ca. 380 K. [C(NH2)3]2HgI4 yielded four 127I NQR lines ascribable to m = ±1/2 ? ±3/2 transitions, indicating that its crystal structure is different from the bromide complex. The 1H NMR T 1 measurements showed a single minimum for the bromide but two minima for the iodide. The analyses based on the C3 reorientations of the planar [C(NH2)3]+ ions gave the activation energies of 29.8 kJ mol?1 for the bromide, and 30.2 and 40.0 kJ mol?1 for the iodide. 相似文献
94.
Tomohisa Yamashita Shuji Kodama Mikiya Ohto Eriko Nakayama Sumiyo Hasegawa Nobutaka Takayanagi Tomoko Kemmei Akira Yamaguchi Norio Teramae Yukio Saito 《Analytical sciences》2006,22(12):1495-1500
The permeation fluxes of phenol, benzene sulfonate (BS) and benzene disulfonate (BDS) through a porous anodic alumina membrane with the perpendicularly oriented silica-surfactant nanochannel assembly membrane (NAM) were measured in water-ethanol mixture media. The permeation flux depended on solute charges and on solvent composition. As the ethanol ratio increased, the fluxes of BS and BDS increased and the flux of phenol decreased. The results of extraction/elution experiments also depended on the solute charges and the solvent composition. Chromatographic experiments in n-hexane showed that dipole and hydrophobic interactions affect the retention of solutes. Permeation of the solute across the NAM in water-ethanol mixture is likely to be determined by various factors such as dipole interaction, hydrophobic interaction, solvation, and anion-exchange efficiencies. 相似文献
95.
A complete list of Finsler, Scott and Boffa sets whose transitive closures contain 1, 2 and 3 elements is given. An algorithm for deciding the identity of hereditarily finite Scott sets is presented. Anti‐well‐founded (awf) sets, i. e., non‐well‐founded sets whose all maximal ∈‐paths are circular, are studied. For example they form transitive inner models of ZFC minus foundation and empty set, and they include uncountably many hereditarily finite awf sets. A complete list of Finsler and Boffa awf sets with 2 and 3 elements in their transitive closure is given. Next the existence of infinite descending ∈‐sequences in Aczel universes is shown. Finally a theorem of Ballard and Hrbá?ek concerning nonstandard Boffa universes of sets is considerably extended. 相似文献
96.
Atsushi Kubo Thomas P. Spaniol Takehiko Terao 《Journal of magnetic resonance (San Diego, Calif. : 1997)》1998,133(2):330-340
The effect of bulk magnetic susceptibility (BMS) on solid state NMR spectra of paramagnetic compounds was investigated theoretically and experimentally. The BMS shift was calculated for cylindrical and spherocylinderical containers with some ratios of the lengthLand the diameterD. The results show the best resolution can be obtained by using a long cylindrical sample container withL/D> 10 and by exciting only the region near the center of the container. The effect of the random orientations and distributions of crystallites in a powder sample was also calculated according to a model proposed by Schwerket al.[J. Magn. Reson. A119, 157 (1996)] with removing the Fermi contact term from their model. Static and the magic-angle spinning13C NMR spectra were recorded on two paramagnetic compounds of Ln(C2D5SO4)3· 8H2O where Ln = Pr, Yb. The modified theory predicts the BMS broadening of the experimental spectra very well. 相似文献
97.
A urinary glucose assay has been investigated, employing a micro flow injection analysis (microFIA) combined with a separation technique of glucose from the analyte. The adsorption part using activated alumina for the glucose in the analyte can be successively integrated onto a microFI chip. The selective adsorption-desorption of glucose in the artificial urine can progress on the adsorption part. Along with this selective preconcentration of glucose, the typical FI peak of glucose can be obtained just by feeding the sample and deionized water as an elutant sandwiched with the reagent on the carrier stream. The glucose concentration in artificial urine can be quantitatively determined with the present microFIA system, while the interference of other components coexisting in urine occurs in the case of the conventional FIA system without any separation part. The described method serves as a template for improving the selectivity for the analyte in the multi-component system. 相似文献
98.
Yoshitaka Ishii Koichi Hirao Takehiko Terao Tsutomu Terauchi Makoto Oba Kozaburo Nishiyama Masatsune Kainosho 《Solid state nuclear magnetic resonance》1998,11(3-4):169-175
A solid state NMR method is presented for determination of a backbone dihedral angle φ in peptides, being based on the previously reported method, relayed anisotropy correlation (RACO) NMR [Y. Ishii et al., Chem. Phys. Lett. 256 (1996) 133]. In the present method, the
and the
dipolar tensors in the
system are two-dimensionally (2D) correlated via polarization transfer from
to
under magic angle spinning (MAS). This method was applied to N-acetyl
,
-valine, and the H–C–N–H dihedral angle was determined to be 154.0±1.4° or 206.0±1.4°, the former agreeing with the X-ray value of 154±5°. 相似文献
99.
100.
Junichi Goto Nobhuharu Goto Atsuko Hikichi Tomoko Nishimaki Toshio Nambara 《Analytica chimica acta》1980
Two highly sensitive, chiral derivatization reagents, D- and L-1-aminoethyl-4-dimethyl-aminonaphthalene, were synthesized from 1-dimethylaminonaphthalene. Condensation of carboxylic acids with the chiral reagent was readily effected in the presence of a watersoluble carbodiimide. The diastereoisomeric amides formed from N-acetylamino acid and α-arylpropionic acid enantiomers were efficiently resolved by normal phase chromatography (μPorasil column) -with hexane/ethyl acetate or hexane/tetrahydrofuran as a mobile phase. With a fluorescence detector (excitation 320 nm, emission 395 nm), the detection limit was 0.1 ng. 相似文献