BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 41, Issue 12
Displaying 1-14 of 14 articles from this issue
  • Kyoko FUJIMOTO, Teruo OKANO, Yasuharu MATSUMURA
    1992 Volume 41 Issue 12 Pages 609-616
    Published: December 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The determination of trace elements in solid samples has been studied by direct sample insertion ICP-AES. We used a thin-stemmed graphite cup which has small thermal capacity and large thermal conductivity. Trace elements, as low as the ppm level, in organic materials and aluminium nitride could be determined with high accuracy using calibration curves obtained with standard solutions. In order to determine refractory and/or carbide-forming elements with high sensitivity, a halogenation technique for the vaporization of these elements was investigated. Carrier gas including halogenating reagent obtained by bubbling a carrier gas through one of the reagents such as Freon and hydrochloric acid was introduced continuously into the plasma. By this halogenation technique, high sensitivity was attained for these elements (detection limits: 0.1 to 0.3 ng).
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  • Mikita ISHII, Tooru TAKAHASHI, Shinichi BABASAKI
    1992 Volume 41 Issue 12 Pages 617-625
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A natural reddish dye from the red rose petals extracted with 0.5 M sulfuric acid solution was applied to chemiluminescent enhancement of active oxygen produced by neutralization energy of acid-base reaction. Using a flow injection system equipped with the enhancement technique, sulfuric acid of high concentration was rapidly, easily and sensitively determined. The 3 lines are consisted of sodium hydroxide (6 M), octadecyltrimethylammonium chloride (1×10-2 M) and the reddish dye at a flow rate of 3.5 ml/min each. Analytical characteristics of the proposed system are as follows. Magnitude for the determination: 818 M in the 10 μl injection method (S/N=1.5), analytical time required: ca. 10 s, relative standard deviation: 2.0% for 5 repeated runs of the 9 M sulfuric acid solution. The determined values for the proposed system agreed well with those for the conventional method.
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  • Katsutoshi ITO, Masako MAEDA, Akio TSUJI
    1992 Volume 41 Issue 12 Pages 627-632
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    We have developed a sensitive time-resolved fluoroimmunoassay for the determination of human secretin in plasma. Europium(Eu)-chelate labeled antigen was prepared by labeling Eu-chelate {N-(p-isothiocyanatobenzyl)diethylenetriamine-N, N, N, N-tetraacetic acid europium(III)} to secretin-bovine serum albumin conjugate. The assay procedure was as follows: a standard secretin solution or sample (100 μl), rabbit anti human secretin anti-serum solution (50 μl) and Eu chelate labeled antigen solution (50 μl) were added to the well of microtiter plate coated with goat anti rabbit IgG antibody and incubated at 4°C overnight. Then, the wells were washed with 0.05 mol/l Tris-HCl buffered saline containing 0.05% Tween 20 six times. Enhancement solution (200 μl) was added to each well and incubated at room temperature for 10 min. The time-resolved fluorescence intensity was measured. The measurable range for secretin was from 2.5 to 100 pg/assay and the RSD was 0.783.39% (n=8). Cross-reactivities of anti-secretin antiserum with various related peptide hormones were less than 0.01 % of secretin. The extraction of secretin from serum or plasma using Sep-pak C18 cartridge was examined. The recovery of secretin was 74.9±17.9 (mean±SD)%. Immunoreactive secretin levels in normal and obstructive jaundice subjects obtained by the proposed method were 23.3±7.3 pg/ml (n=8) and 54.1±10.9 pg/ml (n=7), respectively.
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  • Yutaka HAYASHIBE, Minoru TAKEYA, Yasumasa SAYAMA
    1992 Volume 41 Issue 12 Pages 633-638
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A flow injection method has been studied for the determination of cobalt in high-salt concentration (zinc electrolyte) solutions to be used for wet refining. The sample solution containing about 150 g Zn l-1 was injected four times into a carrier stream, and the carrier stream was merged with 2 M acetate-0.5 M citrate buffer solution (pH 6) to form a sample solution stream. The colorimetric reagent (1.0% (w/v) nitroso-R salt) was injected into the sample solution stream. Then coexisting metal complexes were decomposed by mixing with 2 M sulfuric acid-1% (v/v) hydrogen peroxide solution. Finally, the absorbance of cobalt complex was measured at 480 nm. Just before the determination of Co, colorimetric reagent alone was injected into the analytical system for the measurement of background absorbance, and the background absorbance was utilized for the correction of the system variation. A calibration curve was constructed by using solutions prepared by adding various increments of the standard cobalt solution to the real sample solution, of which cobalt concentration had been determined by a combined solvent extraction/GF-AAS method. The proposed system was operated automatically by a personal computer and allowed 6 samples to analyze per hour. Precision of the system was a RSD of 8% at the 0.5 μg Co ml-1 level and detection limit was 0.05μg Co ml-1
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  • Soichi OTSUKI, Kimihiro ADACHI
    1992 Volume 41 Issue 12 Pages 639-642
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A film composed of a Rhodamine dye and a hydroxypropylcellulose matrix was investigated for the optical humidity measurement. The film containing Rhodamine 6G (R6G) or Rhodamine B (RB) showed a total decrease of the fluorescence which was 50% and 88%, respectively, with increasing relative humidity. The fluorescence intensity of the R6G-based film showed a reversible response for the repeated RH changes between 0 and 90%, while that of the RB-based film decreased at first and came to be approximately constant during the above repetition of RH change, and after which the latter also showed a reversible response for the RH change between 0 and 90%. It is thought that the decrease in the fluorescence intensity is attributed to the quenching effect of water for both films. The 90% response time of the RB-based film is 6 and 14 min for stepwise humidity changes of 71 to 90% RH and 0 to 32% RH, respectively.
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  • Kimiya OKAZAKI, Masaki MIFUNE, Junichi ODO, Yutaka SAITO
    1992 Volume 41 Issue 12 Pages 643-647
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    To extend analytical application of ion-exchange resins, a ternary salt-like resin, a cation-exchange resin (Amberlite CG-50) on which oxyzirconium ion and tetrakis(sulfophenyl)porphine (TPPS) were loaded, was prepared. The ternary resin (R-Zr·TPPS) reacts with fluoride ion to liberate TPPS. Since the amount of released TPPS corresponds to that of fluoride ion, fluoride ion can be determined spectrophotometrically. It was found that the result was the most satisfactory, when the ternary resin was prepared by loading 53.4 mg of zirconium oxynitrate and 25 mg of TPPS on 1 g of CG-50 and then washing the resin with diluted nitric acid (1 M and 0.1 M). The calibration curve obtained was linear in the range of 1 to 5 ppm fluoride ion. The relative standard deviation (n=10) was satisfactory (2.2 % ). R-Zr·TPPS was expected to be useful as a new conceptional reagent.
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  • Katsumi UCHIYAMA, Junichi MINOWA, Yoshihiro YOSHIMURA, Takaho WATANABE ...
    1992 Volume 41 Issue 12 Pages 649-653
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Photoacoustic determination of sodium dodecyl sulfate was proposed by the use of solid-phase concentration method with Empore plate. Sodium dodecyl sulfate was extracted as a Methylene Blue complex in chloroform according to JIS K 0102. Aqueous sample containing trace amount of anionic surfactants (0300 μg) was determined. The chloroform extract was filtered through the Empore plate (2.5 cm squares) with self-made suction filtering apparatus. Interfering methylene azures were eluted through the plate. The plate was cut into 13 mm circle and then photoacoustic signal was measured. By the pretreatment of the plate with sodium bicarbonate, the blank signal intensity was decreased to the half of the one without treatment. Linear relationship was obtained between the concentration of anionic surfactant and the photoacoustic intensity in the range 0500 ppb. Detection limit of anionic surfactant was approximately 3.6 ppb. Using river waters as samples, the analytical results were nearly equal to those by the JIS method. A five hundred nanograms of anionic surfactant was added to the river water to test the recovery. The recovery of anionic surfactants was in the range of 98.099.6%.
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  • Shigeaki YONEMORI, Hideshi SASAKURA, Kumiko TAGUCHI
    1992 Volume 41 Issue 12 Pages 655-658
    Published: December 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Chemical degradation method of ester-type polyurethanes composed of polyesterpolyols, polycaprolactonepolyols, or polycarbonatepolyols was investigated. Pyridine containing water was an effective reagent to hydrolyze urethane bond selectively without cleaving ester bond. One gram of polyurethane sample was heated at 160°C in a mixture of 10 ml of pyridine and 0.5 g of water in a pressure vessel. Urethane bond was completely hydrolyzed after 15 h under this condition. After evaporating the reagent, the molecular weight and composition of the polyols were determined by GPC and NMR. In the case of polycarbonates, a lower decomposition temperature of 130°C was preferable to avoid the cleavage of carbonate bond.
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  • Nobuo NAKANO, Yoshio KOBAYASHI, Kunio NAGASHIMA
    1992 Volume 41 Issue 12 Pages 659-661
    Published: December 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A quantitative method, using tapes which have been impregnated with silver nitrate (AgNO3) has been used in the detection of hydride gases such as phosphin and arsine. The hydride gas is absorbed on the surface of the tape and reacts with the silver nitrate to form a stain and the intensity of which can be measured quantitatively by an optics system to determine the concentration of the gas. Silver nitrate is extremely light sensitive and unstable. The tape coated with silver p-toluenesulfonate (AgC7H7SO3) is more stable to light (about 1500 lx) and retains a white background for five times as long as the tape coated with silver nitrate. The sensitivity of the tape coated with silver p-toluenesulfonate for phosphin and arsine is nearly equal to that of the tape coated with silver nitrate.
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  • 1992 Volume 41 Issue 12 Pages e1
    Published: 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • Minato ANDO, Takashi KATO, Tunetoshi OKURA, Yasuyuki MIZUSHIMA, Junich ...
    1992 Volume 41 Issue 12 Pages T141-T144
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A practical liquid-lens cell was constructed. 1, 1, 2-trichlorotrifluoroethane was the most suitable liquid as a liquid-lens material. This liquid in the aluminium pipe is heated by the exothermic decomposition of hydrogen peroxide in the catalytic reactor and the beam diameter of incident light is reduced. This light beam diameter decreased to 20 μm when the concentration of H2O2 was 8 mM. Reduction of the light beam diameter was roughly correlated with hydrogen peroxide concentration.
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  • Hideaki KINOSHITA, Toshiaki USUI, Yoshiaki KANEDA, Tokuji IKEDA
    1992 Volume 41 Issue 12 Pages T145-T149
    Published: December 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Oligosaccharide dehydrogenase-modified graphite paste electrode containing benzoquinone produced biocatalytic current due to the oxidation of glucose and oligosaccharides. The magnitude of the current due to the saccharide was inversely proportional to the amount of glucose in the saccharide. The current produced by the solution containing maltopentaose and serum, in which maltopentaose was hydrolyzed to maltose and maltotriose, gradually increased with the time, and the increase in current was proportional to the amount of serum. The increase in current by the solution of low activity of amylase was very small and this method was not adequate for the measurement of such samples. The addition of 100 U ml-1 α-glucosidase to the solution containing 2 mM maltopentaose and serum diluted 1/30, gave α current increase for 10 min of 7 times as compared with a solution not containing α-glucosidase. Amylase activity in human serum measured with this electrode in the presence of α-glucosidase agreed well with that by a photometric method which is used in many hospitals (r=0.974, n=13)
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  • Yoshinori UWAMINO, Hisashi MORIKAWA, Akira TSUGE, Kiyoshi NAKANE, Yasu ...
    1992 Volume 41 Issue 12 Pages T151-T156
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Several sample decomposition methods were examined to determine trace impurities in sintered silicon carbide and silicon nitride. The pulverized samples were severely contaminated. A lump (about 0.15 g) of sintered silicon carbide sample was decomposed with a mixture of 5 ml of sulfuric acid+2.5 ml of nitric acid+2.5 ml of hydrofluoric acid in a Teflon pressure vessel at 230°C. Similarly about 0.3 g of sintered silicon nitride sample was decomposed with a mixture of 6 ml of nitric acid+4 ml of hydrofluoric acid at 170°C. The proposed methods were applied to some commercial samples, and the impurities were determined by ICP-AES.
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  • Toshiya OGIWARA, Shigeo TANUMA
    1992 Volume 41 Issue 12 Pages T157-T161
    Published: December 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    We have investigated the dependence of the depth resolution in Auger sputter depth profiling on sputtering ion energy using Ni/Cr multilayer thin film specimen. The used ion species for sputtering was Ar. The accelerating voltages were 0.5, 1.0, 2.0, 3.0 kV. The measured Auger lines were Ni-MVV, Ni-LMM, Cr-LMM. The depth resolution of all Auger lines were proportional to the square root of sputtering ion energy. The main reason for the widening of the interface width with high energy ion beam might be due to the surface roughness caused by ion bombardment. When the Auger depth profile analysis of Ni/Cr multilayer thin film were carried with the Ar ion 0.5 kV, the depth resolution of Ni-MVV, Ni-LMM, Cr-LMM did not depend on the depth of the sample.
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