Determination of trace water in highly purified nitrogen by low temperature adsorption/GC method.

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  • 低温吸着濃縮／ガスクロマトグラフィーによる高純度窒素中の微量水分の定量
  • テイオン キュウチャク ノウシュク ガス クロマトグラフィー ニ ヨル コウ

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Abstract

It is very difficult for conventional analytical methods to determine trace water in highly purified nitrogen. In this study, a low temperature adsorption/GC was applied to the determination of the water in nitrogen. The water was adsorbed and condensed in columns filled with Porapak T and cooled to about 3°C. Adsorbed water was released by heating the columns and was detected by a gas chromatograph equipped with TCD. The peak area was proportional to water concentration from 0 to above 0.6 ppm and the detection limit was about 0.02 ppm. Water in nitrogen(S-grade extra pure, steel cylinder), in nitrogen(for semiconductor process, aluminium cylinder with High-Coat treatment), in nitrogen balanced ethane(10.5 ppm, steel cylinder) and in nitrogen balanced acetylene(10.5 ppm, steel cylinder) was determined. Coexistent ammonia (975 ppm), ethane and acetylene did not interfere with the determination. Water concentrations at room temperature were about 0.3 ppm for nitrogen(S-grade) and 0.1 to 0.2 ppm for the other gases. Dependences of water concentration on cylinder temperature and on inner pressure were observed. Water concentration increased as the temperature increased and/or the pressure decreased.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 36 (4), 267-270, 1987

    The Japan Society for Analytical Chemistry

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