Rapid and Simultaneous Micro-analysis of Halogens and Sulfur in Organic Compounds by Combustion - Ion Chromatography

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  • 燃焼イオンクロマトグラフィーによる有機化合物中のハロゲン及び硫黄の高速一斉分析
  • ネンショウ 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 ハロゲン オヨビ イオウ ノ コウソク イッセイ ブンセキ

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Abstract

A method for the rapid and simultaneous micro-analysis of organic halogens and sulfur that employs a novel coupled combustion - ion chromatography (IC) apparatus is described in detail. The cost has been decreased by switching from argon (helium) - oxygen for the carrier gas to cleaner air. In addition, a standard sample that contained 4 halogens and sulfur was developed concerning the making of calibration curves. A sample of 1.0–10 mg (micro) or 0.1–1.0 mg (ultra-micro) was weighed and ignited in a quartz combustion tube at 1000 °C. The combustion products were collected in a 40 mL (total volume) of mixed solution of very tin hydrogen peroxide and hydrazine hydrate. After a 50 μL aliquot of each sample solution was injected into a suppressed conductivity IC system. The calibration curves of the peak areas of each element (F, Cl, Br, I and S) were obtained from the combustion standard (NAC-st4: C12H7NO2FClBrIS) with high correlation coefficients (r2) of more than 0.999. The 5–6 samples per one hour were able to be analyzed by this combustion/IC system within 0.3 % of the theoretical values.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 66 (2), 81-87, 2017

    The Japan Society for Analytical Chemistry

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