Determination of antimony by a combination of evolution-separation with X-ray fluorescence spectrometry

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Other Title
  • アンチモンの気化分離‐けい光Ｘ線分析法による定量
  • アンチモン ノ キカ ブンリ ケイコウ Xセン ブンセキホウ ニヨル テイリョ
  • アンチモンの気化分離-けい光X線分析法による定量

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Description

A method was presented for the determination of antimony in pig lead. The method consisted of the evolution of stibine, its fixing on a chloroauric acid. test paper, and the measurement by X-ray fluorescence spectrometry.<BR>Procedure: Transfer a sample solution containing up to 200μg of antimony into an evolution vessel (200-ml Erlenmeyer flask). Add 15 ml of 12 M hydrochloric acid, and dilute the mixture to 50 ml with water. Add 5 g of granular zinc, and immediately connect a capture vessel to which a test paper has been attached. After standing for an hour, remove the test paper, set it on a sample holder, and count the X-ray fluorescence intensity of the SbKα line (2θ=13.47°) in a vacuum using a tungsten target X-ray tube (50 kV-20 mA) and a LiF crystal.<BR>The intensity of the X-ray fluorescence was almost proportional to the antimony amount (up to 200 μg). The standard deviation was 2.6% (with 100 μg of antimony) in five runs.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 25 (1), 65-67, 1976

    The Japan Society for Analytical Chemistry

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