Organic elemental analysis using a microbomb

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  • KONDO Asaji
    Laboratory of Organic Chemistry, Tokyo Institute of Technology

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Other Title
  • ミクロボンベによる有機元素分析(III)
  • ミクロボンベ ニ ヨル ユウキ ゲンソ ブンセキ 3
  • Gravimetric microdetermination of organic selenium
  • 有機セレン微量重量定量

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Abstract

A simple microdetermination of organic selenium has been investigated. The sample in a microbomb is decomposed by the sodium peroxide method in a short time; the product of decomposition is taken up in water ; the hydrogen peroxide present in the solution is decomposed by gentle boiling with a platinum foil; and the solution is neutralized with conc HCl. The solid suspension is filtered off, and the solution is adjusted to contain 34 N HCl. Aqueous hydrazine solution is added to reduce the selenous acid produced by the decomposition, precipitating it as a red selenium. This is converted to a black selenium by heating it for more than 30 min, and letting it stand overnight. The selenium is filtered off through a no. 4 glass filter, pried and weighed. Even the presence of N, S, halogens (including iodine) does not interfere with the determination of selenium by this method. The errors of analyses were ± 0.5 % of theory.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 6 (9), 583-585, 1957

    The Japan Society for Analytical Chemistry

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