Determination of trace manganese in high-purity selenium by a combustion-kinetic method

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  • FUKASAWA Tsutomu
    Department of Applied Chemistry, Faculty of Engineering, Yamanashi University
  • YAMANE Takeshi
    Department of Applied Chemistry, Faculty of Engineering, Yamanashi University
  • YAMAZAKI Takeshi
    Department of Applied Chemistry, Faculty of Engineering, Yamanashi University

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Other Title
  • 揮散分離‐反応速度法による高純度セレン中の極微量マンガンの定量
  • キサン ブンリ ハンノウ ソクドホウ ニヨル コウ ジュンド セレンチュウ ノ
  • 揮散分離・反応速度法による高純度セレン中の極微量マンガンの定量

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Abstract

A simple and sensitive method has been developed for the determination of manganese in high-purity selenium. Selenium was expeled mainly as selenium dioxide by being heated in a quartz boat (net volume, ca. 2 ml) in an electric furnace at 600°C in air stream of 150 ml per min. for 35 min. Expeled selenium dioxide was absorbed in a water trap. Combustion of sample at lower temperature (below ca. 500°C) was time-consuming and was liable to product red-selenium. After the complete separation of selenium, the combustion boat was taken out from the furnace and cooled to room temperature. The residue in the boat was dissolved in 0.5 ml of 6M hydrochloric acid and the solution was gently evaporated to dryness on a hot-plate. Then manganese in the residue was dissolved in an acetate buffer solution (pH 3.8) and was determined by the catalytic method based on the oxidation of Malachite Green by periodate, as previously described. The conditions of combustion and others were studied in detail. The proposed method allows the determination of manganese as low as 10 ppb for 1 g of sample.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 26 (3), 200-202, 1977

    The Japan Society for Analytical Chemistry

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