X光谱分析法在测定萤石硫中的应用

Application of X-fluorescence spectrophotometric in the determination of sulfur in fluorite

萤石中硫的检测方法有硫酸钡重量法、红外线吸收法、燃烧碘量法、ICP法，因硫酸钡重量法耗时长且不易操作；燃烧碘量法出现较高含硫量的萤石样时燃烧不完全、低含量的样品终点颜色易滴定过量；用红外吸收法测定时，因氟离子的腐蚀导致碳硫仪气路管和金属过滤器堵塞，影响仪器的正常运行和数据出现较大偏差。本文介绍了利用x荧光压片法测定萤石中的硫，用ICP—AES电感耦合等离子体发射光谱法和x荧光光谱法进行比对，结果精密度和准确度较高。

The detection methods of sulfur in fluorite include barium sulfate gravimetrie method, infrared absorption method, combustion iodometry and ICP method, barium sulfate gravimetric method is time-consuming and difficult to operate, the combustion of fluorite with high sulfur content is not complete by the method of combustion iodometry, and the terminal color of the sample with low content is easy to be titrated in excess, when measured by infrared absorption method, the corrosion of fluorine ion leads to the blockage of the gas pipe and metal filter of the carbon sulfur meter, which affects the normal operation of the instrument and results of large deviation. This paper introduces the determination of sulfur in fluorite by means of X-ray fluorescence tablet method, and the comparison between inductively coupled plasma emission spectrometry and X-ray fluorescence spectrometry is carried out by ICP-AES, results the precision and accuracy are high.