ガスクロマトグラフィーによる重水素濃度の高感度迅速定量法

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タイトル別名
  • Rapid and sensitive determination of deuterium concentration by gas chromatography
  • ガス クロマトグラフィー ニ ヨル ジュウスイソ ノウド ノ コウカンド ジン

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抄録

Gas chromatographic determination of hydrogen isotopes D2 and HD has hitherto been carried out with a molecular sieve column kept at -195°C under the H2 carrier gas. However, the amount of D2 in hydrogen gas containing low HD concentration of less than 5 % can be practically neglected judging from the equilibrium constant of H2-D2exchange reaction. Therefore, there is no need to separate HD from D2. As an improvement, in this paper, the gas chroma tographic determination of HD in low concentration (<5%) was carried out by maintaining the temperature of the molecular sieve 13X column at room temperature. Since HD passed freely through the column under this condition, rapid analysis became possible. Moreover, the use of ultra pure H2 as a carrier gas enabled us to enhance the cell current of TCD drastically, hence gave rise to high sensitivity of HD detection. The limit of determination of the concentration of HD was 0.01%. In the case of the higher concentration (>5%) of HD in hydrogen gas, D2 and HD have been separated and determined by the method described above, but this method takes more than ten minutes. Therefore, we designed a new gas chromatographic analysis of the HD-D2 mixture with an activated alumina column at -195 °C under the H2 carrier gas (330 ml/min). The advantages of this method are in (1) rapid analysis (in 1 min), (2) no need of the rigid activation temperature {(110250) °C}, (3) no change of the relative molar sensitivity of HD to D2 at the various flow rates of H2 carrier gas {(100300) ml/min}.

収録刊行物

  • 分析化学

    分析化学 33 (2), 104-107, 1984

    公益社団法人 日本分析化学会

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