惰气熔融-红外吸收/热导法同时测定无烟煤中氮和氢

Simultaneous Determination of Nitrogen and Hydrogen in Anthracite by Inert Gas Melting-Infrared Absorption/Thermal Conductivity Method

  • 摘要: 首次使用惰气熔融-红外吸收/热导法实现无烟煤中氮、氢元素的同时、快速、准确测定. 探究分析条件,发现当称样量为0.030 0 g,分析功率为5 500 W,氮元素的积分延迟时间为15 s,集成时间为55 s,氢元素的积分延迟时间为5 s,集成时间为85 s,且使用石墨套埚时,氮氢元素的释放最完全、合理. 方法中氮、氢校准曲线的相关系数分别为0.994 9、0.994 0,检出限分别为0.321%、0.189%,定量限分别为0.326%、0.194%,精密度分别为3.60%、0.63%,满足线性关系及方法要求. 惰气熔融-红外吸收/热导法重复性好、高效便捷、操作和维护简单,可用于无烟煤中氮、氢元素的定量检测.

     

    Abstract: The contents of nitrogen and hydrogen in anthracite were simultaneously, rapidly and accurately determined by the inert gas melting-infrared absorption/thermal conductivity method. A series of experiments were studied. The results indicated that the most complete and reasonable release of nitrogen and hydrogen was achieved when the sample was 0.030 0 g, the analysis power was 5 500 W, the integration delay time of nitrogen was 15 s, the integration time of nitrogen was 55 s, the integration delay time of hydrogen was 5 s, the integration time of hydrogen was 85 s, and the graphite sleeve crucible was used. The correlation coefficients of calibration curves of nitrogen and hydrogen were 0.994 9 and 0.994 0, respectively. The limits of detection were 0.321% and 0.189%, the limits of quantification were 0.326% and 0.194%, and the precision were 3.60% and 0.63%, respectively, which met the requirements of linearity and method. The inert gas melting-infrared absorption/thermal conductivity method is reproducible, efficient and convenient, easy to operate and maintain, and can be used for the quantitative determination of nitrogen and hydrogen in anthracite.

     

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