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

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0.0300 g,分析功率为5500 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0.9949、0.9940,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.

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 0.0300 g,the analysis power was 5500 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 0.9949 and 0.9940,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.