熔融制样-X射线荧光光谱法测定硫化铜钼矿中主成分

Determination of major components in sulfide copper-molybdenum ore by X-ray fluorescence spectrometry with fusion sample preparation

建立了熔融制样-X射线荧光光谱法测定硫化铜钼矿中铜、钼、铁、硫、二氧化硅、氧化钙等主成分的分析方法。选择熔融制样作为前处理手段，通过观察试验现象、分析各待测元素响应情况以优化实验参数。确定取样量为0．4000g，氧化剂硝酸锂用量为2．0000g，混合熔剂四硼酸锂／偏硼酸锂（m：m=67：33）用量为6．0000g，预氧化时间为8min，熔融时间为8rain，双向摆动熔融时间为4＋2min，脱模剂为溴化锂的熔融条件。混合铜矿石、钼矿石国家标准物质配制具有浓度梯度的校准样品序列，保证校准曲线线性范围涵盖硫化铜钼矿选矿流程样品中各目标成分的含量分布区间。方法检出限分别为14（铜）、24（钼）、85（铁）、31（硫）、56（二氧化硅）、70（氧化钙）μg／g。对2个混合样品进行了分析，测定值与参考值相符，结果的相对标准偏差（n：10）在0．09％～0．68％之间。

A determination method for the major components such as copper, molybdenum, iron, sul- fur, silicon dioxide and calcium oxide was established by X-ray fluorescence spectrometry with fusion sample preparation. The experimental parameters were optimized through observing experimental phenomenon and analyzing the responses of each element with sample fusion preparation. It was de- termined that 0. 400 0 g of sample amount, 2. 000 0 g of oxidizer LiNO3, 6. 000 0 g of mixed flux Li2B4OT/LiBO2（m ： m=67 ： 33）, 8 min pre-oxidation, 8 min fusion, 4-1-2 min two-way swing fusion and LiBr release agent was adopted. Copper ore and molybdenum ore national certified reference mate- rials were mixed to prepare calibration sample series with content gradient to ensure the linear range of calibration curve cover the whole distribution range of target element in the beneficiation samples of sulfide copper-molybdenum ores. The detection limit was respectively 14 （Cu）, 24 （Mo）, 85 （Fe）, 31（S）, 56 （SiO2）, 70 （CaO） μg/g. Two mixed standard samples were analyzed and the results were compared with the reference values. The relative standard deviation （n=10） was 0. 09 %-0. 68 %.