BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 41, Issue 6
Displaying 1-10 of 10 articles from this issue
  • Susumu SHIMOYAMA, Yasuko NODA
    1992 Volume 41 Issue 6 Pages 243-250
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    For the determination of the natural dyestuffs used for an ancient coloring cloth without damage of the cloth, the three-dimensional fluorescence spectrum of each standard sample was measured to draw a contour plot diagram of fluorescence intensity upon the coordinate of the excitation (λEx) vs. emission wavelength (λEm). It was found that the dyestuffs can be identified by the respective top ring of contour line showd by both wavelength as follows : (A) Dyestuff from the plant Rubia cordifolia L. var. Munjista Miq. root, “Akane” in Japan, λEx 409419 nm/λEm 599619 nm; (B) from the plant Miscanthus tinctorius Hackel leaf, “Kariyasu”; λEx 442466 nm/λEm 522538 nm ; (C) from the plant Gardenia jasminoides Ellis berry, “Kuchinashi”; λEx 409424 nm/λEm 529557 nm; (D) from the sea invertebrate Rapana thomasiana hypobranchial gland, “Akanishi”; λEx 335352 nm/λEm 432441 nm; (E) from the plant Polygonum tinctorium Lour. leaf, “Tadeai”, λEx354370 nm/λEm 404416 nm; (F) from the plant Carthamus tinctorius L. petal, “Benibana”; λEx 547570 nm/λEm 592605 nm.
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  • Sadao MORI, Yasuhiko NISHIMURA
    1992 Volume 41 Issue 6 Pages 251-255
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The identification of polymers having no UV absorption and the discrimination of blends composed of two homopolymers from the copolymers having the same composition have been performed by HPLC system, using silica gel as the stationary phase, a refractomer as a detector, and several solvents such as chloroform and ethyl acetate as the mobile phases. Sample polymers were polystyrene (PS), polyvinyl chloride (PVC), polyvinyl acetate (PVAc), and several polymethacrylates and polyacrylates. Sample polymers were dissolved in tetrahydrofuran which was a good solvent for these polymers in a 0.1% concentration and the injection volume of these sample solutions was 0.1 ml. Identification was based on the elution of polymers from or the retention of polymers in the column and not on the difference in retention volumes. PVC eluted with the mobile phase of 1, 2-dichloroethane (DCE) and PVAc was retained in a column. The methanol mobile phase showed opposite results. The blends of PVC and PVAc were discriminated from the P(VC-VAc) copolymers with the mobile phases of DCE and methanol.
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  • Shinkichi YAMADA, Noriyoshi OHTO, Motoshi NAKAMURA, Shigeru NAKAMURA
    1992 Volume 41 Issue 6 Pages 257-261
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The kinetics and thermodynamics of the complexation reactions of aluminium, gallium and indium with morin have been studied fluorometrically to find the tolerance level for aluminium in the kinetic determination of gallium and indium. Under the selected conditions in which the pH of the reaction solution and the concentration of morin are 2.3 and 1×10-4 M, respectively, the differences in formation rates and fluorescent intensities for the respective complexes allow kinetic separation of gallium and indium from aluminium. The more reactive gallium or indium was selectively determined by a linear extrapolation method in the presence of aluminium; gallium and indium could be determined up to 1×10 -5 M with a detection limit of 9×10 -9 M and up to 5×10 -6 M with a detection limit of 2×10-8 M, respectively. In the determination of 5×10 -7 M of gallium and indium, the presence of a 400- and 500-fold amount (by molarity) of aluminium could be tolerated, respectively.
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  • Kazuhisa YAMAYA, Toshiyuki AOKI, Il Yong KIM
    1992 Volume 41 Issue 6 Pages 263-268
    Published: June 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A hydride generation methed is studied for preconcentration of trace amounts of selenium prior to AAS measurements. The procedure is as follows ; Transfer 40 cm3 of sample solution and 20 cm3 of hydrochloric acid to a reaction vessel and inject 3% NaBH4 solution with a flow rate of 3 cm3 min -1 for 45 s. Hydrogen selenide is generated from the sample solution by passing nitrogen at a flow rate of 125170 cm3 min -1 for 20 min. The nitrogen gas bearing the H2Se-gas is introduced into an absorbing solution (3 mol dm -3 HClO4 15 cm3+ +0.02 mol dm -3 KMnO4 0.25 cm3+ 0.05 mol dm -3 sodium oxalate 0.15 cm3) through a sintered glass filter (2030 μm). Then transfer it into 100 cm3 beaker and add 3 cm3 of nitric acid. Heat on a hot plate at 160°C to evaporate solwly to about 23 cm3. Then add 10 cm3 of 6 mol dm -3 HCl to the solution and heat to about 125°C for 3045 min for reduction of Se(VI) to Se(IV). The selenium contents of the concentrated samples were determined by AAS with hydride generation. By the proposed method, 0.030.75 ng cm -3 of selenium can be quantitatively recovered and determined with the precision of ± 0.01 ng cm -3 (95% confidence interval).
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  • Masaki KATOH, Tamio KAMIDATE, Hiroto WATANABE
    1992 Volume 41 Issue 6 Pages 269-274
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A chemiluminescence(CL) method was developed for the determination of inorganic phosphorus by using the hydrogen peroxide generated from the enzymatic reaction with inorganic phosphorus. Phosphorylation of inorganic phosphorus was done by nucleoside phosphorylase and was coupled with the generation of hydrogen peroxide with xanthine oxidase at pH 7.4. Hydrogen peroxide was subsequently determined by the CL of the mixed solution of bis(2, 4, 6-trichlorophenyl)oxalate-perylene reagent containing a surfactant. The CL intensity depended upon the buffer components and the charge-type of surfactants. The CL intensity was greater in 0.05 M imidazole buffer solution than that in 0.05 M Tris buffer solution. The best sensitivity was achieved by using a cationic surfactant, hexadecyltrimethyl chloride. Analytical calibration curve was prepared under the optimized experimental conditions. Logarithmic calibration curve of inorganic phosphorus was linear from the detection limit of 5.0×10-8 M up to 1.0×10 -5 M. The relative standard deviation was 2.7% at 2.0×10 -6 M inorganic phosphorus. Proteins such as albumin reduced the CL intensity, but their interference was simply avoided by the dilution of serum by a factor of 100 with the imidazole buffer solution. The present method was applicable for the determination of inorganic phosphorus in serum.
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  • Kazuya YAMASAKI, Masayuki KIKUOKA, Takafumi SAEKI, Yoshio KOKUSENYA, M ...
    1992 Volume 41 Issue 6 Pages 275-279
    Published: June 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    HPLC with electrochemical detection using enzyme reaction was developed for determination of lecithin in gastric juice. In this method, lecithin extracted from gastric juice was hydrolyzed by phospholipase D. The liberated choline was injected to HPLC and separated by reverse phase column and converted to betaine and hydrogen peroxide (H2O2) by column packed with immobilized choline oxidase. H2O2 was detected by electrochemical detector. The detection limit for lecithin was 2 ng/injection. The peak area of HPLC was proportional to the concentration of lecithin from 0.1 to 1.5 μg/ml. The relative standard deviation was 1.88% (n=6). The coefficient of lecithin recovery from human gastric juice was 97.0% (n=3).
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  • Hiroshi KAWAMOTO, Wataru ISHIDA, Kin-ichi TSUNODA, Hideo AKAIWA
    1992 Volume 41 Issue 6 Pages 281-283
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Ammonium ion reacts with 4, 7, 13, 16, 21, 24-hexaoxa-1, 10-diazobicyclo[8.8.8]hexacosane, Cryptand(2.2.2), to form ammonium cryptate which is quantitatively extracted into chloroform as vermilion complex with dithizone. In this work the resulting vermilion complex was utilized for the spectrophotometric determination of ammonium ion. Twenty five milliliters of an aqueous solution containing ammonium ion was shaken with 25 cm3 of chloroform containing 1.0×10-3 mol dm -3 Cryptand(2.2.2) and 4×10-5 mol dm-3 dithizone in a separatory funnel. The mixture was shaken for 10 min by a mechanical shaker. After phase separation, the absorbance of the chloroform phase at 496 nm and the pH value of the aqueous phase were measured. The extracted species had a molar absorptivity of 1.0×104 dm3 mol-1 cm-1 at the absorption maximum of 496 nm. As Na+, K+ and several heavy metals were expected to interfere with the extraction process, a distillation step was introduced to remove these metal ions. A linear calibration curve was obtained up to 1 μg cm-3, the detection limit of the present method being 0.13 μg cm-3 of ammonium ion. The relative standard deviation of the measurements was 1.4% for 0.60 μg cm-3 ammonium ion standard solution. The present method was successfully applied to the analysis of several river water samples.
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  • Yoshinobu AKADA, Eiji KAWAKAMI
    1992 Volume 41 Issue 6 Pages 285-287
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A rapid and simple determination of acrinol (2-ethoxy-6, 9-diaminoacridine monolactate) in pharmaceutical preparations was investigated by FIA. The sample solution was injected into the carrier stream (water), merged with 0.5% potassium nitrite and 0.5% hydrochloric acid and then passed through a 10 m reaction coil (0.5 mm i.d.) at room temperature. Absorbance was measured at 517 nm. There was a linear relationship (r =0.999) between peak height and concentration of acrinol. The proposed method was successfully applied to the determination of pharmaceutical preparations.
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  • Shogo SUZUKI, Shoji HIRAI
    1992 Volume 41 Issue 6 Pages T87-T90
    Published: June 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Trace elements in iron and steel certified reference materials, JSS 002-3 (Pure Iron), JSS 003-2 (Pure Iron) and JSS 814-1 (Iron Ore), prepared by the Iron and Steel Institute of Japan were determined by instrumental neutron activation analysis (INAA). Six aliquots of each sample (ca. 100750 mg) were irradiated for a short time (30 s) at a thermal neutron flux of 1.5×1012 n cm-2 s-1 and for a long time (6 h) at a thermal neutron flux of 5.5×1011 n cm-2 s-1 in the Rikkyo University Research Reactor. After a suitable decay-period, these irradiated aliquots were measured by two γ-ray spectrometries; a conventional counting method using a coaxial Ge detector, and an anticoinicidence counting method using a coaxial Ge detector and a well type NaI(Tl) detector. Eight elements in JSS 002-3, 13 elements in JSS 003-2 and 35 elements in JSS 814-1 were determined by these methods. The determined values were in good agreement with the certified and reference values of 412 elements.
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  • Hisomu NAGASHIMA, Takeshi OHTSUKA, Akinori ISOZAKI
    1992 Volume 41 Issue 6 Pages T91-T96
    Published: June 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A simplified suppressor using a cation exchange membrane tube (Dionex AFS-2) with a conductometric detector has been developed for ion chromatography (IC). The method to prepare the suppressor is described below. A 500-ml polyethylene bottle was drilled many holes to pass the membrane tube smoothly and some large squared holes to make exchange easy between aqueous solutions inside and outside of the bottle. The cation exchange membrane tube was passed through the holes inwards and outwards alternately, like sewing, surrounding the bottle many times. The drilled bottle was immersed in a scavenger solution stirred by a stirrer in a 1-1 beaker. Determination of inorganic anions was performed with the simplified suppressor-IC ; column, TSK gel IC-Anion-PWXL (porous polymethacrylate gel) : eluent, 3 mM NaHCO3-0.8 mM Na2CO3 solution: flow rate, 1.2 ml/min : column temp., ambient. When a 25 mM sulfuric acid solution was used as a scavenger, the best chromatograms were obtained and the relative standard deviations (R.S.D.) of peak heights of the standard mixed ion solution (F-, Cl- NO2-, Br-, NO3-, HPO42-, SO42- and I-) were 0.6 to 1.2% (8 anions, n=12). The present method was satisfactorily applied to simultaneous microanalysis of chlorine and sulfur in organic compounds, after the oxygen flask combustion. The analytical values were in good agreement with the theoretical ones for any compound examined within an error of ±0.3 %.
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