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Keihei UENO
1988 年 4 巻 4 号 p.
337
発行日: 1988年
公開日: 2007/07/27
ジャーナル
フリー
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Tsugio KOJIMA
1988 年 4 巻 4 号 p.
338
発行日: 1988年
公開日: 2007/07/27
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Hiroshi KAWAGUCHI
1988 年 4 巻 4 号 p.
339-345
発行日: 1988/08/10
公開日: 2006/06/27
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Inductively coupled plasma-mass spectrometry is a rapidly growing technique for multi-elemental analysis. In this review, instrumental developments, analytical performance and applications of this method achieved recently are described. Ion sampling interface, ion lens systems and various sample introduction systems are discussed. Suppression of analyte signals is usually observed in the presence of matrix salts at high concentration; this effect is generally more serious than those observed in inductively coupled plasma atomic emission spectrometry. The dependency of the suppression effect on the atomic weight of matrix elements is discussed. Applications to real samples for the determination of trace elements and isotope ratios are described.
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Osamu YAMAMOTO, Kikuko HAYAMIZU, Masaru YANAGISAWA
1988 年 4 巻 4 号 p.
347-352
発行日: 1988/08/10
公開日: 2006/06/27
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A data file structure of a
1H-NMR database with a full spectral pattern is described together with the registration procedure. The
1H-NMR data file comprises two master and one access files. One of the master files is a data file for a digitized spectral pattern (MASTER FILE II) and the other includes information concerning the spectrum (MASTER FILE I). For both files, some expenditures are made to compress the data for the reduction of the memory size in the database. An example of output of a
1H-NMR spectrum is given. The problems in constructing the
1H-NMR database system are discussed.
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Yoshio KOSUGI
1988 年 4 巻 4 号 p.
353-355
発行日: 1988/08/10
公開日: 2006/06/27
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Carbon-13 NMR spectra of a number of
m- and p-substituted benzenesulfonic acids in basic deuterium oxide solutions have been obtained. Simple additivity rules for chemical shifts are totally useless for all carbons except for several carbons in
p-CH
3,
p-Et, and
p-Cl derivatives. Deviations of a few ppm have been rationalized for 1, 3- and 1, 4-disubstituted benzenes, but deviations of 7ppm are the largest among C-13NMR chemical shifts data so far reported. The astonishing deviations are observed at the carbon attached to sulfo anion and at both adjacent carbons. The nature of the sulfo group changes according to the second substituent; it is not regulated by the substituent parameters which include various kinds of sigma values.
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Shigekazu TSURUBOU
1988 年 4 巻 4 号 p.
357-360
発行日: 1988/08/10
公開日: 2006/06/27
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The formation constants of the adducts formed between quinine or quinidine and bis(3-trifluoroacetyl-d-camphorato)copper(II), bis(3-heptafluorobutyryl-d-camphorato)copper(II), or bis(3-pivaloyl-d-camphorato)copper-(II) have been determined spectrophotometrically in carbon tetrachloride, benzene, toluene,
m-xylene, chloroform and 1, 2-dichloroethane. The formation constant of quinine adduct is always greater than that of quinidine one in each bis(3-acyl-d-camphorato)copper(II)-organic solvent system so far examined.
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Masanosuke TAKAGI, Junji KOJIMA, Naofumi MORITA
1988 年 4 巻 4 号 p.
361-364
発行日: 1988/08/10
公開日: 2006/06/27
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L-α-Glycerophosphate oxidase was fixed on the surface of an oxygen electrode by keeping the enzyme in a glutaraldehyde-linked membrane. The current response of the sensor was linear with the concentration of glycerophosphate in the range of 0.05 to 1.5mM. The relative correlation coefficient was 0.999 (
n=5). The response time was about 2min. The standard deviation of ten measurements with 0.8mM glycerophosphate in buffer pH 7.5 was 3.8%. The electrode was stable for at least 30d. However, reducing materials such as L-ascorbic acid gave rise to some error.
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Sadao MORI
1988 年 4 巻 4 号 p.
365-369
発行日: 1988/08/10
公開日: 2006/06/27
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Low- and high-conversion styrene-methyl methacrylate random copolymers, P(S-MMA), were fractionated by size exclusion chromatography (SEC). Each fraction was subjected to liquid adsorption chromatography (LAC) using silica gel as an adsorbent and a mixture of chloroform and ethanol as the mobile phase. In low-conversion P(S-MMA), the differences of peak composition of LAC chromatograms for SEC fractions were 4-5% and the difference between the highest and the lowest styrene content in components was about 10%. CCD became broader with decreasing molecular size. One sample of low-conversion P(S-MMA) showed two peaks in a LAC chromatogram, showing that this sample was a mixture of two copolymers of different compositions. LAC peaks of SEC fractions for high-conversion P(S-MMA) were broad compared to low-conversion ones; the difference of peak composition for one sample was 11% and the range of composition was between 21 and 52% styrene. LAC is a very useful technique for obtaining CCD of copolymers and compositional differences in a sample.
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Kunihiko DOHTSU, Kiyoshi OHMORI, Ryuji FUKUDA, Shigeori TAKENAKA, Mako ...
1988 年 4 巻 4 号 p.
371-376
発行日: 1988/08/10
公開日: 2006/06/27
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The use of intercalator-nucleic base stacking interactions is developed and experimentally examined for the separation of mononucleotides and oligonucleotides by high performance liquid chromatography (HPLC). Silica gel chromatographic supports were modified with anthracene- and phthalimide-containing groups. The chromatographic supports so obtained were used for the separation of mononucleotides and pentadecamer oligonucleotides under reversed-phase, isocratic conditions. The separation behavior was studied in comparison with that using standard octadecylsilyl-modified silica gel (ODS) support. Separation among nucleotides was quite different for intercalator-based supports and for the ODS support, suggesting the importance of stacking
interactions of anthracene and phthalimide groups with nucleic bases. Directions for the development of HPLC supports based on such interactions are discussed.
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Kazutake SHIMADA, Tomoyuki OE, Chiyomi KANNO, Toshio NAMBARA
1988 年 4 巻 4 号 p.
377-380
発行日: 1988/08/10
公開日: 2006/06/27
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Cyclodextrin was used as a component of mobile phase for the separation of cardenolides by reversed-phase high performance liquid chromatography. The addition of γ-cyclodextrin to the mobile phase improved the separation of isomeric cardenolides. The proposed method was applied to the isolation of cardiac glycosides having a doubly linked sugar from plant material and to the clarification of ring C ketol rearrangement products of cardiac glycosides.
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Hidenao TOYODA, Kazufusa SHINOMIYA, Shigeyuki YAMANASHI, Ichiro KOSHII ...
1988 年 4 巻 4 号 p.
381-384
発行日: 1988/08/10
公開日: 2006/06/27
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A highly sensitive high performance liquid chromatographic method with fluorometric postcolumn labeling using 2-cyanoacetamide was developed for determination of unsaturated disaccharides produced enzymatically from chondroitin sulfates (ChS). The calibration curves of the unsaturated disaccharides were linear over the range from 2pmol to 5nmol. This method was applied to the analysis of normal rabbit plasma for ChS to verify the sensitivity and practicality.
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Masaharu NAKAJIMA, Akira SATO, Kenji SHIMADA
1988 年 4 巻 4 号 p.
385-388
発行日: 1988/08/10
公開日: 2006/06/27
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A sensitive method for the determination of serum valproate by HPLC with fluorometric detection has been developed. Valproate was led to acid chloride with thionyl chloride, which in turn was transformed with 9-aminophenanthrene (9-AP) into the amide derivative. The 9-AP-derivatized valproic acid exhibited excitation and emission maxima at 303nm and 376nm, respectively. The derivative was subjected to HPLC on a Shimpack CLC-ODS column (150×6mm i.d.) with methanol-acetonitrile-water (23:11:6) as the mobile phase. The detection limit of the method was 9.4pg for valproic acid (VPA). The method was successfully applied to the determination of serum VPA of epileptic patients. The satisfactory correlation was observed between the results obtained by the present method and enzyme immunoassay.
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Mitsunori MURAYAMA, Masao SUZUKI, Shoji TAKITANI
1988 年 4 巻 4 号 p.
389-392
発行日: 1988/08/10
公開日: 2006/06/27
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A method for the determination of selenium by ion chromatography (IC) after oxygen flask combustion has been developed and applied to the determination of selenium in bulk prednisolone. We found elemental selenium [Se(0)], selenite ion [Se(IV)] and selenate ion [Se(VI)] (ca. 5, 75 and 20%) in the absorbing liquid obtained by oxygen flask combustion of Se(0), Se(IV) and Se(VI). Se(VI) was directly determined by IC. Se(IV) was determined as Se(VI) after oxidation by potassium permanganate. Se(0) was oxidized to Se(VI) by hydrogen peroxide and potassium permanganate. In this method, the recovery of selenium was in the range of 95-100%, and the detection limit was 63ng (79pg with concentrator) in 40mg of sample.
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Hajime KARATANI
1988 年 4 巻 4 号 p.
393-398
発行日: 1988/08/10
公開日: 2006/06/27
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The polymer effect of the copolymer of 4-vinylpyridine and
N-vinylpyrrolidone(prepared by radical polymerization) on the Chemiluminescence of a 5-amino-2, 3-dihydro-1, 4-phthalazine dione/hydrogen peroxide/copper(II) system in an alkaline solution was studied. This was done to apply the polymer effect to the chemiluminescence determination of trace copper(II). The luminol chemiluminescence catalyzed by copper(II) was strongly enhanced in the presence of the copolymer. This seemed to be attributed to the increase in the catalytic activity of copper(II) due to the polymer effect. Furthermore, the effect of the copolymer on the luminol chemiluminescence has been applied to the determination of copper(II) at the ppb concentration level by the use of the flow method.
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Atsushi SUGII, Naotake OGAWA, Kumiko HARADA, Koichi NISHIMURA
1988 年 4 巻 4 号 p.
399-402
発行日: 1988/08/10
公開日: 2006/06/27
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Poly(4-vinylpyridine), 4VP, resins cross-linked with oligo(ethylene glycol dimethacrylates) were used for chelating resins. Sorption for some metal ions by complexation in acetate buffer (pH 3-6) was investigated mainly by using the 4VP resins cross-linked with hydrophilic tetraethylene glycol dimethacrylate (4VP-4EG) and that cross-linked with hydrophobic divinylbenzene (4VP-DVB). The difference in cross-linkers of the 4VP resins strongly affected the sorption behavior, such as the pH profile of the sorption of metal ions and the capacity for Co(II), Ni(II) and Cu(II). 4VP-4EG showed higher metal sorption than 4VP-DVB in acetate buffer, suggesting that hydrophilicity of the resin matrix, other than chelating groups, should be taken into account in the design of chelating resins.
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Tadashi MOCHIZUKI, Akiko SAKASHITA, Hideo IWATA, Takako KAGAYA, Tadash ...
1988 年 4 巻 4 号 p.
403-409
発行日: 1988/08/10
公開日: 2006/06/27
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The results of a preliminary study on direct analysis of solid metals and nonconductive samples by inductively coupled plasma mass spectrometry (ICP-MS) are described. The aerosols ablated from solid samples by a ruby laser are introduced into an inductively coupled plasma, with detection of the resulting ions by a mass spectrometer. With conventional solution introduction, polyatomic species from mineral acids and solvents prevent the accurate determination of some trace analytes. However, using laser ablation, these background peaks are greatly reduced. The relative sensitivity factors for the laser ablation method are seen to vary from unity, with volatile elements such as Pb and Bi being more sensitive. Detection limits of rare-earth elements, Th and U in silicate rocks are excellent (0.02-0.9ppm at the effective integrating time of 1.4s), being better than those of the examined elements in steel (1.7-29ppm at the effective integrating time of 0.6s).
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Tatsutoshi KANETAKE, Makoto OTOMO
1988 年 4 巻 4 号 p.
411-415
発行日: 1988/08/10
公開日: 2006/06/27
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The spectrophotometric characteristics of the complexes formed with di-2-pyridylmethanone 2-(5-nitro)pyridylhydrazone (DPNPH) and eight metal ions are reported. The reagent appears to be promising especially for palladium(II) and cobalt(II) in selectivity and for copper(II), nickel(II), zinc(II) and cadmium(II) in sensitivity. A detailed study has been made for the extractive spectrophotometric determination of up to 2.8ppm of palladium(II) in the presence of chloride ions. The molar absorptivity of the complex extracted into 1, 2-dichloroethane is 3.78×10
4l mol
-1 cm
-1 at 560nm. The method is satisfactorily applied to the determination of palladium in some palladium catalysts.
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Joichi UEDA, Chika MIZUI
1988 年 4 巻 4 号 p.
417-421
発行日: 1988/08/10
公開日: 2006/06/27
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The trace amounts of gallium and indium in water were determined by graphite furnace atomic absorption spectrometry after being concentrated by the coprecipitation technique with hafnium hydroxide. Hafnium hydroxide coprecipitates quantitatively 0.2-3μg of gallium from 50-400ml of sample solution at pH 6.0-10.5 and 0.2-4μg of indium from 50-400ml at pH 6.0-11.0. The atomic absorbances of gallium and indium are increased about 3 times by the presence of hafnium; the reproducibilities of the measurements are also improved. The calibration curve is linear from 8 to 120ng ml
-1of gallium or from 8 to 160ng ml
-1of indium. Twenty seven diverse ions tested did not interfere seriously with either element. These methods are applicable to the determination of gallium and indium in river or seawater which contains down to 0.5ng ml
-1of these elements.
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Shunichi UCHIYAMA, Yoshinobu TOFUKU, Shuichi SUZUKI, Giichi MUTO
1988 年 4 巻 4 号 p.
423-424
発行日: 1988年
公開日: 2007/07/27
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Hiroshi OGINO, Yoko AOMURA, Taketoshi SUZUKI, Masahiko HATANO
1988 年 4 巻 4 号 p.
425-426
発行日: 1988年
公開日: 2007/07/27
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Isao KOJIMA, Tetsuo UCHIDA, Chuzo IIDA, Kouichi IEDA, Takeo MUKAI
1988 年 4 巻 4 号 p.
427-428
発行日: 1988年
公開日: 2007/07/27
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Yukio NAGAOSA
1988 年 4 巻 4 号 p.
429-430
発行日: 1988年
公開日: 2007/07/27
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Yuko YAMASHOJI, Takahiro KAWAGUCHI, Takayuki MATSUSHITA, Masanori WADA ...
1988 年 4 巻 4 号 p.
431-432
発行日: 1988年
公開日: 2007/07/27
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Keiji GAMOH, Takao YAGI
1988 年 4 巻 4 号 p.
433-435
発行日: 1988/08/10
公開日: 2006/06/27
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