为解决钼精矿标准分析方法步骤繁琐、1 次只能测定 1 种元素的问题,开发了一种分析速度快、溶样方法简单且适用于钼精矿中多种元素同时测定的分析方法.该方法采用基体分离方式,利用电感耦合等离子体发射光谱法(ICP-OES)对钼精矿中多种元素进行测定;使用双氧水-盐酸-硝酸-高氯酸强氧化体系溶解钼精矿,去除矿物中的碳和浮选剂等物质,然后通过过滤将三氧化钼沉淀从样品溶液中与铼分离,有效消除基体干扰.在发射功率 1.2 kW、辅助气流速 1.0 L/min、雾化气流速 0.7 L/min、蠕动泵泵速 12 r/min条件下,对溶液酸度、基体及共存元素的干扰进行了探究.结果表明,工作曲线线性相关系数均>0.999,检出限为 0.000 3~0.02 μg/mL,相对标准偏差为 0.82%~4.96%.该方法与钼精矿国家标准分析方法相比,对钼精矿标准物质GBW(E)070212 和GBW(E)070213 的分析结果基本一致.
In order to solve the problem that the standard analysis method of molybdenum concentrate has complicated steps and can only measure one element at a time,an analysis method was developed that has fast analysis speed,simple sample dissolution method and was suitable for the simultaneous determination of multiple elements in molybdenum concentrate.Inductively coupled plasma emission spectrometry(ICP-OES)was used to determine various elements in molybdenum concentrate by ma-trix separation.The research mainly dissolves molybdenum concentrate in a strong oxidation system of hydrogen peroxide-hydrochloric acid-nitric acid-perchloric acid to remove substances such as carbon and flotation agents from the mineral.Then,effectively eliminated matrix interference by separating molybdenum trioxide precipitation from rhenium in the sample solution.Under the conditions of transmitting power of 1.2 kW,auxiliary gas flow rate of 1.0 L/min,atomizing gas flow rate of 0.7 L/min,and peristaltic pump speed of 12 r/min,the interference of solution acidity,matrix and coexisting elements were studied.The results show that the linear correlation coefficients of the work-ing curve are greater than 0.999,the detection limits are 0.000 3~0.02 μg/mL,and the relative standard deviations are 0.82%~4.96%.The analysis results of GBW(E)070212 and GBW(E)070213 for molybdenum concentrate are basically consistent with those of the standard analysis method.