高频燃烧-红外吸收光谱法测定钼矿石和镍矿石中的高含量硫

高频燃烧-红外吸收法用于分析矿石中低含量硫的测定结果较为准确,但对于高含量的硫,分析结果的准确度不高。本文采用高频燃烧-红外碳硫分析仪测定钼矿石和镍矿石中的高含量硫,选择纯铁屑和钨粒作助熔剂,高温燃烧分解样品,通过实验优化了样品称样量、助熔剂用量、仪器分析时间等测定条件。用国家标准物质进行验证,方法精密度(RSD,n=9)小于1%,加标回收率为96.0%～101.9%;与传统的硫酸钡重量法进行比对试验,测定值的相对误差小于2%。针对不同的矿石样品,研究了实际样品与标准物质的基体匹配问题,消除了基体效应的影响,对于钼矿石和镍矿石样品中含量在1%～35%范围内的硫,均能够准确测定,解决了钼矿石和镍矿石中高含量硫的快速、准确测定问题。

Determination of High Content Sulfur in Molybdenum Ore and Nickel Ore Using High Frequency Combustion-Infrared Absorption Spectrometry

By using the high frequency Infrared Absorption Spectrometric method, the determination of low levels of sulfur in ores was accurate; but not for the high sulfur content. High content sulfur in molybdenum ore and nickel ore was determined by CS-3000 High Frequency Combustion-Infrared Absorption Spectrometer in this study. The samples were burned at high-temperature and decomposed by adding the flux of the pure ion filings and tungsten grains. The measurement conditions such as sample amount, the quantity of flux and analysis time of the instrument have been optimized. The method was verified by national standard materials, the precision was less than 1% (RSD, n=9) and the sample recoveries ranged from 96.0% to 101.9%. Compared with the conventional barium sulfate gravimetric method, the accuracy of the method is less than 2% (relative error). The study focused on the matrix matching problem between samples and standard materials, and the influence of the matrix effect. The tests show that the content of sulfur between 1% and 35% in molybdenum ore and nickel ore can be determined accurately. The problem for the rapid and accurate determination of high content sulfur in molybdenum ore and nickel ore was solved.