超级微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定乌兰茶晶石中15种稀土元素含量

Determination of 15 REEs in Ulan Citrine by Inductively CoupledPlasma Optical Emission Spectrometry (ICP-OES) with Super Microwave Digestion

乌兰茶晶石富含稀土型矿物,准确测定乌兰茶晶石中的稀土元素含量具有非常重要的意义。通过15组微波消解试剂条件实验及对超级微波消解仪工作参数的优化,最终确定采用硝酸-氟硼酸-磷酸体系在超级微波消解仪中260℃下加热30 min进行样品消解,赶酸后用2%硝酸复溶,建立了超级微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定乌兰茶晶石中15种稀土元素的方法,整个过程高效、操作简便、无损失、无污染。利用ICP-OES进行测定,所选谱线无干扰、信背比高,校准曲线线性相关系数大于0.99995,测试结果准确,相对标准偏差<4.0%,加标回收率在91.3%~96.3%。方法用于花岗岩(GBW07103)测试,测定值与标准值一致。结果表明,硝酸-氟硼酸-磷酸消解法可替代碱熔法对乌兰茶晶石实际样品进行前处理,具有较好的稳定性和准确性,能满足实际应用需求。

Ulan citrine is the rare earth elements(REEs)bearing mineral.It is of great significance to accurately determine REEs in Ulan citrine for its application in the ceramic industry.In this paper,through 15 groups of digestion reagent condition experiments and optimization of the working parameters of the super microwave digestion,the HNO 3,HBF 4 and H 3 PO 4 were finally selected to dissolve the Ulan citrine samples during super microwave digestion process(heating at 260℃for 30 min),and 2%HNO 3 was added after acid-drying.This paper established a method for the determination of REEs in Ulan citrine by inductively coupled plasma optical emission spectrometry(ICP-OES),the whole process was efficient,easy to operate,no loss and no pollution.In addition,the selected spectral line was measured without interference,the signal-to-background ratio(I/I b)was high,the linear correlation coefficient of the calibration curve was greater than 0.99995,the precision was<4.0%,and the results of recovery test was between 91.3%and 96.3%.This method was applied in the determination of REEs in the national geochemistry standard reference materials-GBW07103,and the measured values were consistent with the standard values.In conclusion,this method can replace the alkali fusion method to pretreat the actual samples of Ulan citrine,and it has better stability and accuracy,which can meet the practical application needs.