BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 16, Issue 2
Displaying 1-14 of 14 articles from this issue
  • Hideo NAGAI, Ikuko YAMASAKI
    1967 Volume 16 Issue 2 Pages 95-99
    Published: February 05, 1967
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    By increasing the solubility of precipitates in the precipitation chromatography, some developers with limited compositions were found to give a high separability of bands and a minimized band contamination, combining the feature of the precipitation chromatography and the soluble type chromatography. The authors named this procedure as "low solubility chromatography".
    On a sheet of 9cm circular filter paper impregnated with 8mg oxine, a drop of sample solution saturated with iso-butanol was developed at 20°C with a 3:2 mixture of 1% acetic acid and dioxane saturated with oxine. The result was good for the separation of lanthanum and other ions. The mutual separation of the latters, however, was done satisfactorily by employing an oxine-impregnated filter paper which diminished to half the content of the reagent.
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  • Hiroshi HIRATA, Toshioki AMEMIYA, Kenji DATE
    1967 Volume 16 Issue 2 Pages 99-103
    Published: February 05, 1967
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Rapid determination of zinc in grease was investigated by fluorescent X-ray spectrography. Two equal quantities of a sample were weighed out. One was dissolved in dithizone-chloroform solution, and the other in zinc-dithizone-chloroform solution. Two pieces of filter paper were separately soaked in each solution and dried. The amount of zinc in the sample was calculated from fluorescent X-ray intensities of these filter papers using standard-addition-method.
    The method was applied to the analysis of samples containing 0.007 to 0.24% of zinc, and the results were in good agreement with those by chemical method. The time required for an analysis was about forty minutes.
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  • Study of trace elements in food. I
    Sadaji FURUTANI
    1967 Volume 16 Issue 2 Pages 103-110
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A high frequency polarographic method for simultaneous determination of zinc and cobalt or zinc and nickel has been studied in tetramethylammonium bromide supporting electrolyte. Application of the high frequency of 100kc among 50kc, 100kc, 250kc, 500kc and 1000kc gave a good result, and calibration curves were linear in the range of 5×10-7 to 2.6×10-5M for zinc, 5×10-6 to 1×10-4M for cobalt and nickel, respectively. It is possible to determine zinc coexisting with 100 times of cobalt and nickel in 0.5M supporting electrolyte solution at 100kc and H. F. voltage 0.6V. In the case of cobalt and nickel in solution containing zinc, the amounts of zinc must not exceed 10times of nickel and 5times of cobalt.
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  • Hajime ISHII
    1967 Volume 16 Issue 2 Pages 110-114
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The spectrophotometric method for the determination of titanium with diantipyrylmethane has been studied in order to be applied to the determination of a small amount of titanium in cements and their raw materials (cement raw mixture, limestone, gypsum and clay). The procedures have been established on the basis of the results obtained from all-over reexamination on fundamental conditions for the determination. Titanium in the samples described above was able to be determined with satisfactory accuracy and reproducibility. It was found further that the method with diantipyrylmethane was superior for the determination of titanium in these samples to the conventional methods, for example, the method by hydrogen peroxide.
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  • Kazuhisa KOMURA, Masanobu SAKANOUE
    1967 Volume 16 Issue 2 Pages 114-118
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Separation of long-lived radionuclides which belong to uranium and actinium series was investigated by using an anion exchanger resin Dowex 1-X 8. Radioactive tracers (237U, 233Pa, 234Th, 224Ra and 59Fe) were prepared by proper methods and used for examining the chemical behaviors of these elements on anion exchange resin. It was confirmed by a batch method that radium was not adsorbed on the oxalate form resin, while uranium, protactinium, thorium and iron were strongly adsorbed on the resin from various concentrations of oxalic acid solution (0.020.5M). So, the separation of radium from these elements can be easily realized by passing oxalate solution through the column and washing with 0.5M oxalic acid solution. Stepwise separation of adsorbed elements was studied by various eluents. Thorium can be eluted by passing 8N HCl solution through the column, converting the resin form from oxalate to chloride. Then, by adding hydrofluoric acid to the eluent, protactinium can be easily eluted. Separation of uranium from iron had been difficult because of the similar behaviors of both elements on chloride form resin, but it was successfully accomplished by using a mixed medium of 6N HCl-1N HClO4 as an eluent. Iron is adsorbed strongly on the column by this procedure. The consecutive separation method mentioned above is very simple and useful for the geochronological studies of fossil carbonate samples, uranium minerals, peat, etc.
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  • Manki KOMATSU, Teisuke OKANO
    1967 Volume 16 Issue 2 Pages 118-122
    Published: February 05, 1967
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Non-destructive, fractional determination of resibufogenin and bufalin by a universal-type, automaticrecording liquid chromatograph with thermal detection equipment was carried out together with fundamental examination on the analytical conditions. A fractional characteristic curve for the identification of two steroids and a linear calibration line through the origin were obtained by following the analytical conditions below. Separation column: 0.8φ×50cm. detection column: 0.8φ×10cm, flow-rate: 0.38ml/min., chart speed: 30mm/hr., sensitivity: ±0.01° cfs, temp. of detector: 30°C, room temp.: 2627°C, amount of sample: 1030mg, adsorbent: 100200 mesh silica gel, and both sample solvent and developing solvent: acetone-chloroform-cyclohexane (3:3:4).
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  • Yoko SHIBUYA, Eisuke NISHIYAMA, Kenjiro YANAGASE
    1967 Volume 16 Issue 2 Pages 123-128
    Published: February 05, 1967
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The determination of sulfur in heavy oils by X-rays fluorescence analysis was investigated by using scattered X-rays as the internal standard. The carbon-hydrogen ratio, contaminating elements in heavy oils such as vanadium, nickel, copper, iron, sodium, chlorine, oxygen, nitrogen, etc. and water gave some influences on SKα intensity. It was found, however. that the effects of matrix elements, unevenness of sample surface and change of instrumental conditions on SKα intensity were remarkably reduced by using the scattered X-ray as the internal standard. For the range of 1.07% to 4.15% sulfur in heavy oil, a simple calibration curve was obtained in terms of sulfur content against intensity ratio of SKα/WLβ. Determination of sulfur in heavy oil referring to this calibration curve gave standard deviation of 0.0180.049 % against the value by conventional chemical analysis.
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  • Kazuaki KAWABUCHI, Tetsuya KIRIYAMA
    1967 Volume 16 Issue 2 Pages 128-132
    Published: February 05, 1967
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method was described for the determination of tin and zinc in copper alloys. After the sample had been dissolved in a mixture of nitric and hydrochloric acids together with a small amount of hydrogen peroxide, the obtained solution was treated with sulfuric acid to remove lead by filtration. The filtrate was diluted to a definite volume with water and adjusted to 3N in sulfuric acid. An aliquot of the solution was taken and placed on the top of an ion exchange column of strong basic anion exchanger Dowex 1-X8 in a thiocyanate form. Metal ions such as nickel, aluminum, manganese were first removed with 30ml of 0.5N sulfuric acid, while tin, zinc and copper were retained on the column. Both tin and zinc were subsequently eluted with 15ml of 0.5M NaCl-0.5M NaOH solution. Small amounts of copper tended to contaminate the fraction of tin and zinc and interfered with the determination of both metals. However, this difficulty could be effectively eliminated by masking the copper with thiourea. Tin in effluent was determined photometrically with dithiol and zinc was titrated chelatometrically with EDTA using xylenol orange as an indicator.
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  • Jitsuo SUGITA, Yukio IMAI
    1967 Volume 16 Issue 2 Pages 133-134
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A simple method for the determination of organic halogen compounds has successfully been established by using a combination of thin layer chromatography techniques and oxygen-flask combustion methods. A zone appeared on the silica gel thin layer plate was raked onto the filter paper carrier and the halogen content in the zone has been determined by oxygen-flask combustion method.
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  • [in Japanese], [in Japanese], [in Japanese]
    1967 Volume 16 Issue 2 Pages 135-141
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1967 Volume 16 Issue 2 Pages 142-149
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1967 Volume 16 Issue 2 Pages 150-161
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1967 Volume 16 Issue 2 Pages 165-166
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1967 Volume 16 Issue 2 Pages 166-168
    Published: February 05, 1967
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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