Elemental micro-analysis of fluorine, chlorine, bromine, iodine and sulfur in organic compounds by ion chromatography.

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  • NAGASHIMA Hisomu
    Analytical and Metabolic Research Laboratories, Sankyo Co., Ltd.
  • ORITA Shouzo
    Analytical and Metabolic Research Laboratories, Sankyo Co., Ltd.
  • KUBOYAMA Kazuo
    Analytical and Metabolic Research Laboratories, Sankyo Co., Ltd.

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Other Title
  • イオンクロマトグラフィーによる有機化合物中のフッ素，塩素，臭素，ヨウ素及び硫黄の元素微量分析
  • イオン クロマトグラフィー ニ ヨル ユウキ カゴウブツチュウ ノ フッソ エ

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Description

A method for simultaneous microdetermination of fluorine, chlorine, bromine, iodine and sulfur in organic compounds by ion chromatography (IC) was developed. Sample solutions for IC were prepared according to an oxygen flask combustion method or to dissolution of dissociable halides and sulfate. The following procedure is employed: One to eight milligrams of organic samples were decomposed in the presence of oxygen, in a 500 ml quartz flask for fluorine determination and in a Pyrex flask for other elements. The combustion products were absorbed in 20 ml of 2 mM sodium hydroxide plus 100 μl of 5% hydrazine solution for analysis of all four halogens, and in 20 ml of 2 mM sodium hydroxide plus 100 μl of 1 % hydrogen peroxide solution for analysis of both sulfur and halogens except for iodine. The absorbed solutions were treated with a Toyo pak IC-SP cartridge, and the filtrates were injected into a chromatograph (Yokogawa Electric Works, Model IC 100) equipped with a porous polymethacrylated gel column (TSKgel IC-Anion-PW, at 40°C), a cation exchange membrane suppressor and a conductivity monitor. A 3 mM NaHCO3-1.2 mM Na2CO3 solution was used as a mobile phase at a flow rate of 1.6 ml/min. Calibration curves in the peak area constructed from the sodium or potassium salts of five anions (F-, Cl-, Br-, I- and SO2-4) showed good linearity and high reproducibility over a wide range of concentration. The developed method was successfully applied to the simultaneous elemental micro-analysis including iodine determination. The analytical values were in good agreement with the theoretical values for each compound within an error of ±0.3%.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 38 (8), 378-382, 1989

    The Japan Society for Analytical Chemistry

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