摘 要

    针对氢同位素气体H2、HD与D2之间难以定量分析，本研究对常规气相色谱仪做了改进，使用固定相为改性氧化铝的双填充柱在液氮温度(77.4 K)下分析H2、HD与D2的定量组成。考察了桥流、检测温度、载气流量、进样量与不同载气因素对H2、HD与D2保留时间、峰形与信号灵敏度的影响。实验结果表明：在桥流180 mA、检测温度120℃、氦载气流量110 cm3/min与进样量0.1 mL的检测条件下，该分析系统可以使H2、HD与D2的保留时间分别缩短至66 s、79 s与94 s，并得到较好的峰形与定量结果。

     关键词 氢同位素 固定相，改性氧化铝，保留时间

    Analysis of Hydrogen Isotopes with Gas Chromatography

    Chu Xiaozhong1， Zhou Yaping1， Zhou Li*2， Kou Dengming3

    (Department of Chemistry, Tianjin University, Tianjin 300072)

    (School of Chemical Engineering Research Center, Tianjin University, Tianjin 300072)

    (School of Chemistry, Nankai University, Tianjin 300071)

    Abstract Hydrogen isotopes, H2, HD and D2, are difficult to be separated and quantified with conventional gas chromatographs. Amelioration was, therefore, made using twin packing columns of modified alumina immersed in liquid nitrogen, and the influence of bridge current, detection temperature, carrier gas flow rate, injection amount and the sort of carrier gas on the retention time, shape of peak and signal sensitivity were investigated presently. It was shown that the modified chromatography and the selected analysis condition, namely, bridge current 180 mA, detection temperature 120℃, He carrier gas flow rate 110 cm3/min and injection amount 0.1 mL, produced the retention time 66 s, 79 s and 94 s for H2, HD and D2, respectively, and the peaks have a good shape. As a result, reliable quantitative results were obtained. ......