熔融制样–X射线荧光光谱法同时测定铀钼矿中主次成分

Simultaneous Determination of Major and Minor Components in Uranium-molybdenum Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation

采用混合熔剂熔融制样，建立了同时测定铀钼矿中U，Mo，SiO2，Fe2O3，Al2O3等的X射线荧光光谱法。以Li2B4O7–LiBO2作为熔融试剂，NH4NO3作为样品的氧化剂，样品与熔剂的质量比为1∶10。除使用铀矿石国家标准物质外，主要选取人工混合校准样品及历年实验室比对的铀钼矿校准样品绘制成工作曲线。采用理论系数法校正样品的基体效应，用BrKα，ZrKα，ULα，BaLα，ZnKα谱线扣除相应元素的谱线重叠干扰。该方法各组分测定结果的相对标准偏差均小于2.0%(n=10)；用标准物质验证方法的准确度，测定值相对误差在0.00～8.00%之间，与标准值基本吻合。该法应用于生产实验中，可以满足对铀钼矿准确、快速的测量要求。

A method for simultaneous determination of U, Mo, SiO2, Fe2O3, Al2O3 etc. in uranium-molybdenum ores by X-ray fluorescence spectrometry using fusion sample preparation with mix flux was developed. Li2B4O7–LiBO2 was used as mixed flux, and NH4NO3 was used as oxidizing agent, the mass ratio of samples with mixed flux was 1∶10.Except adding some uranium ore national standard substances, working curve was made by selecting artificial mixture of calibration samples and calendar year laboratory comparison of uranium molybdenum calibration sample. Matrix effects were corrected by the method of theoretical coefficients and the overlapping spectral line interference of the corresponding elements was deducted by Br Kα, Zr Kα, U Lα, Ba Lα, Zn Kαspectral lines. The precision of each component was less than 2.0% (n=10), the method with the relative error of 0.00–8.00% was applied to the determination of these components in national standard material and the results were in agreement with certified values. This method can meet the requirements of accurate and rapid measurement of uranium molybdenum ore in the production experiment.