BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 45, Issue 8
Displaying 1-12 of 12 articles from this issue
  • Hitoshi WATARAI
    1996 Volume 45 Issue 8 Pages 725-744
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Recent advances in kinetic studies on the solvent extraction mechanism were reviewed including the historical background, advances in experimental methods, recent findings concerning extraction kinetics in chelate extraction, ion-association extraction and synergic extraction systems. Kinetic studies in micelle and microemulsion systems were included as well. Interfacial adsorptions, interfacial reactions, diffusion-limited processes and aqueous-phase complexation reactions were especially addressed. The relationship between the extraction rate and separation analysis was also discussed. The importance and role of interfacial phenomena in extraction kinetic mechanisms was stressed.
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  • Yuji MAKITA, Katsumi UCHIYAMA, Toshiyuki HOBO
    1996 Volume 45 Issue 8 Pages 745-751
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    A novel chemiluminescent (CL) method for non-selective detection of organic compounds has been developed by means of photocatalysis of semiconductor thin film. ZnO was used as the semiconductor photocatalyst for the generation of organic peroxides derived from analyte organic compounds in a photochemical reactor. The photochemical reactor cell was prepared by Sol-Gel coating of ZnO on the inside-surface of a Pyrex glass capillary. The production of organic peroxides from organic compounds in the sample solution is induced under illumination by near UV light. CL was generated when bis(2, 4, 6-trichlorophenyl)oxalate (TCPO) was oxidized by the organic peroxides. Therefore, many kinds of organic compound could be detected by this method, theoretically. As a result, this flow injection analysis (FIA) system achieved the detection of organic acids and amines.
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  • I. Automatic data acquisition
    Seita TANEMURA, Yoshiko MIYAGAWA, Soji MIYAGAWA
    1996 Volume 45 Issue 8 Pages 753-757
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    A simple energy scanning and data acquisition system for nuclear resonance analysis with a narrow resonance is presented. Ion beam energy was scanned by supplying a bias of -30 kV+30 kV on a target holder. Since the proton energy is controlled by the bias voltage without changing the terminal voltage of the accelerator, scattering of data in a γ-ray excitation curve is very small. Details of the energy scanning and the data acquisition are described. Some examples for the depth profiling of nitrogen implanted into metals using the nuclear reaction 15N(p, αγ)12C at 429 keV are shown and compared with the calculated results by a Monte Carlo simulation.
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  • Seita TANEMURA, Yoshiko MIYAGAWA, Soji MIYAGAWA
    1996 Volume 45 Issue 8 Pages 759-763
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    A data analysis computer program to obtain depth profiles from excitation curves of resonance nuclear reaction analysis (NRA) is presented. The target is divided into layers of uniform concentration and the reaction probability in a layer is calculated from a starting depth profile, which is obtained from the raw data, using the normalized error function with Gaussian approximation for the overall energy spread. Gamma ray intensity is obtained as the reaction probability times the concentration and the detection efficiency. Iterative simulation is performed until the deviation of the calculated γ-ray excitation curve from the experimental one becomes satisfactorily small. This leads to a very simple computer program, fast to operate with a small computer. An example of the analysis is presented with an explanation of the program.
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  • Toshiro WATANABE, Naoki HASEGAWA, Akira YAMAMOTO, Shiro NAGAI, Shigeru ...
    1996 Volume 45 Issue 8 Pages 765-770
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Capillary electrophoretic methods have been developed for analysis of the natural anthraquinone pigments (lac and cochineal pigments) for food. Lac and cochineal pigments were not separated by capillary zone electrophoresis (CZE) using 50 mM phosphate buffer nor by micellar electrokinetic chromatography (MEKC) with 20 mM sodium dodecyl sulfate. The pigments were successfully separated by MEKC with 2% butyl acrylate-butyl methacrylate-methacrylic acid copolymer sodium salts (BBMA). However, this method did not give reproducible results on repeated runs. Addition of 1 mM EDTA to the BBMA solution improved the reproducibility. The lac and cochineal pigments extracted from foods (juice and jelly) with solid phase extraction cartridges were analyzed by the developed technique.
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  • Hitoshi KOIZUMI, Kikuo SASAMOTO, Yoshihito SUZUKI
    1996 Volume 45 Issue 8 Pages 771-776
    Published: August 05, 1996
    Released on J-STAGE: January 15, 2010
    JOURNAL FREE ACCESS
    The optimum separation conditions for five aromatic amines by capillary zone electrophoresis was described. Citrate/phosphate buffer solution was used as the running buffer. The operational conditions were optimized for five aromatic amines as follows: capillary, 700 mm (effective length: 500 mm)× 50 μm i.d. fused silica capillary; buffer solution, 25×10-3 moll-1 citrate/phosphate buffer (pH 4.5); applied voltage, 10 kV (142 Vcm-1); capillary temperature, 40°C; detection wavelength, 205 nm. Five aromatic amines could be completely separated within 12 min. In general, better resolution by CZE is obtained with a higher applied voltage. In this experiment, the resolution of aromatic amines was increased when a lower voltage was applied. For this reason, it is concluded that incomplete replacement of sample bands was caused by both increased electroosmotic flow and suppressed dissociation. The repeatability (n=5) of the migration time and the peak area for aromatic amines was better than 0.6% and 9.0% as RSD, respectively.
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  • Hiroyuki KONDO, Akihiro ONO, Takeshi UEMURA, Taka-aki MINAMI
    1996 Volume 45 Issue 8 Pages 777-782
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    A rapid analytical system for steel samples using ICP-AES has been developed. In this system a steel sample is directly dissolved by electrolysis using a flow-through electrolytic cell, and the solution containing dissolved ions is introduced to plasma continuously. After the sample is set on the electrolysis chamber, an automatic sequence proceeds under the control of a personal computer. A sample can be analyzed in about 60 s. Steel samples of Japanese Standards of Iron and Steel were dissolved with controlled current electrolysis in hydrochloric acid (1+1) as the electrolyte, followed by ICP-AES measurement. The analytical results were in good agreement with the certified values except for titanium in a few samples. In order to determine titanium contained in steel in the form of inclusions, which could be hard to dissolve in acid media at room temperature, the composition of the electrolyte solution and electrolytic potential were studied. By electrolyzing the samples in hydrochloric acid-nitric acid mixture (1+1+2) and maintaining the electrolytic potential at 0.81 V (vs. Ag/AgCl reference electrode), titanium contents which were in good agreement with the certified values could be obtained in all the samples examined in this experiment.
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  • Kensuke ARAI, Miyuki KIMURA, Fumiyo KUSU, Kiyoko TAKAMURA
    1996 Volume 45 Issue 8 Pages 783-787
    Published: August 05, 1996
    Released on J-STAGE: January 15, 2010
    JOURNAL FREE ACCESS
    A method for determining drugs consisting of quaternary ammonium salts was developed based on the reaction of quaternary ammonium ion with a divalent anionic dye, bromophenol blue, to form an ion-association complex extractable into ο-nitrophenyloctylether (NPOE). NPOE is non-volatile and much less harmful than the ordinary extraction solvents such as benzene, dichloroethane and chloroform. Benzethonium chloride, benzalkonium chloride and berberine chloride could be extracted quantitatively into NPOE with the above dye at pH 8.6. The complex showed maximum absorbance at 610 nm and was applied to spectrophotometric determination of benzethonium chloride, benzalkonium chloride and berberine chloride. Each calibration curve of benzethonium, benzalkonium and berberine showed good linearity in the range of 5.0×10-7-2.0×10-5 M with a relation coefficient of more than 0.998 and the relative standard deviation was less than 2.5% (n=10). Benzethonium chloride and benzalkonium chloride in various commercial drugs could be determined precisely by this method. It is thus useful for the sensitive and selective determination of drugs of quaternary ammonium ions.
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  • Jun-ichi ITOH, Masashi KOMATA, Prayitno Susant JOKO
    1996 Volume 45 Issue 8 Pages 789-793
    Published: August 05, 1996
    Released on J-STAGE: January 15, 2010
    JOURNAL FREE ACCESS
    A new highly effective preconcentration method of Cu(II) and Ni(II) in water samples which involved the filtration of pyrrolidinedithiocarbamate (APDC) complexes of these metal ions on a micro-membrane filter (MMF, cellulose nitrate, diameter: 4 mm, pore size: 0.45μm) was developed. It was possible to determine metal ions concentrated on the MMF surface by GFAAS in which the MMF was introduced directly into a cup-type graphite cuvette. Over 95% of Cu(II) and Ni(II) were recovered as APDC complexes by the MMF at pH values from 4 to 9. DDTC was also effective for the recovery of Cu(II) and Ni(II); however, some additions such as Zephiramine and/or coprecipitants (excess Cu(II) for Ni(II)) were required for quantitative recovery. The recoveries of other metal ions, Co(II), Pb(II), Mn(II) and Cd(II) were less than 90%. For the MMF direct ashing technique on GFAAS, addition of 20μl of 5% H2SO4/DMF was effective to minimize variation. A 5 ml aliquot of Cu(II) or Ni(II) sample containing less than ppb-level was enough for one analysis. The sensitivities (3×σ of blank solution) was 40 ppt for Cu(II) and 100 ppt for Ni(II). Relative standard deviation (n=6) was 4.7% for Cu(II) and 2.2% for Ni(II). An application of the method for Cu(II) and Ni(II) in river water was also described.
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  • Hiroki SAKURAI, Kichinosuke HIROKAWA
    1996 Volume 45 Issue 8 Pages 795-798
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Palladium and platinum were reduced and precipitated in aqueous solutions by sodium tetrahydroborate, sodium phosphinate and ascorbic acid. Palladium was reduced by sodium tetrahydroborate, sodium phosphinate and ascorbic acid, and Pt by sodium tetrahydroborate. However Pt and Pd could not be individually separated by the active hydrogen which was generated during the reduction of Pd.
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  • Hiroki SAKURAI, Kichinosuke HIROKAWA
    1996 Volume 45 Issue 8 Pages 799-804
    Published: August 05, 1996
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Serenium and tellurium were reduced and precipitated in aqueous solutions by sodium sulfite, sodium phosphinate, tin(II) chloride, ascorbic acid and thiourea. The optimum concentration of HCl for the individual separation of Se and Te was obtained only for sodium sulfite. The other reductants could not be used for this separation.
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  • Tadashi MIYAZAWA, Satoshi OGINO, Kunio NAKAJIMA, Yukio MINAMI
    1996 Volume 45 Issue 8 Pages 805-809
    Published: August 05, 1996
    Released on J-STAGE: January 15, 2010
    JOURNAL FREE ACCESS
    The Drug-of-Abuse One Step Test for the detection of methamphetamine (MA) and amphetamine (AM) in urine was evaluated. The two kinds of test device, one for MA (Device-MA) and the other AM (Device-AM), examined for their sensitivity and specificity. The detection limits of Device-MA and Device-AM were 1μg/ml and 2μg/ml, respectively. Seven compounds related to amphetamine such as methamphetamine, ephedrine, norephedrin, pseudo-ephedrine, methylephedrine, methoxyphenamine and p-hydroxymethamphetamine were found not to cross-react with Device-AM when tested at concentrations up to at least 200μ/ml. But secondary amines such as methoxyphenamine, p-hydroxymethamphetamine, ephedrine and pseudo-ephedrine were found to crossreact with Device-MA at 0.5, 20, 20, 200 μg/ml, respectively. The results obtained for 175 urine samples by the proposed method using the two devices were compared with those by the conventional method (Syva Emit, TLC and GC/MS). Percent agreements between the two methods for urine samples, which are positive for both MA and AM and negative for both MA and AM were 100%. Total percent agreement was 95%.
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