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在半导体材料和电子器件的生产过程中,对氢气的纯度要求越来越高,因此其中的微量杂质(特别是氧)必须进行控制和分析。测定纯氢中氧的方法有气相色谱法,黄磷发光法和原电池法等。就方法灵敏度和能同时测定多种组份而言,应首推气相色谱法。前人大都采用变温浓缩-气相色谱法来分析氢中ppm~ppb 级杂质。我们用自制的热导检测器和气相色谱系统与变温浓缩技术相结合的方法,较好地解决了高纯氢中氧和氮的测定问题。当浓缩取样量为1升时,方法灵敏度对氧来说是30ppb,对氮来说是60ppb。
In the production of semiconductor materials and electronic devices, hydrogen purity is increasingly high, so trace impurities (especially oxygen) must be controlled and analyzed. Determination of hydrogen in pure hydrogen gas chromatography, yellow phosphoric acid method and the original battery method. In terms of method sensitivity and simultaneous determination of multiple components, gas chromatography should be the most important. Most of our predecessors use temperature-gradient condensation - gas chromatography to analyze hydrogen ppm ppb level impurities. We use home-made thermal conductivity detector and gas chromatography combined with variable temperature condensation technology to better solve the determination of oxygen and nitrogen in high-purity hydrogen. The method sensitivity is 30 ppb for oxygen and 60 ppb for nitrogen when the concentrated sample volume is 1 liter.