熔融制样-X 射线荧光光谱法同时测定石煤钒矿中12 种主次成分
核工业230 研究所，长沙 410007
Simultaneous determination of 12 major and minor components in stone coal vanadium ore by X-ray fluorescence spectrometry with fusion sample preparation
LIU Jinliang, ZHANG Xin, SONG Maosheng
Research Institute No. 230, CNNC, Changsha 410007, China
摘要：建立熔融制样-X 射线荧光光谱法同时测定石煤钒矿中V，Ba，SiO2 等12 种主次成分。采用样品与混合熔剂的质量比为1∶10 熔融制样，高温煅烧除去石煤钒矿中的还原性物质，以人工混合标准样品和历年比对的石煤钒矿样品绘制标准工作曲线，采用烧失量-理论系数法校正样品的基体效应，扣除谱线重叠干扰。样品中主次成分的相对标准偏差均小于5.0%(n=10)，用该方法对4 种石煤钒矿管理样品进行测定，相对误差为-4.55%～4.35%，测定值和标准值基本一致。该方法应用于生产实践中，取得良好的测量效果。
Abstract：A method for simultaneous determination of 12 major and minor components of V, Ba and SiO2 etc. in
stone coal vanadium ore by melting sample preparation-X-ray fluorescence spectrometry was established. Samples were
prepared by melting with the mass ratio of sample to mixed flux of 1:10. The reducing substances in stone coal vanadium
ore were removed by high temperature calcination, and the standard working curves were drawn by manual mixing standard
samples and comparison of samples over the years. The matrix effect of samples was corrected by burning loss-theoretical
coefficient method, and the overlapping interference of spectral lines was deducted. The relative standard deviations
of principal and minor components in the sample were less than 5.0%(n
=10). Four kinds of stone coal vanadium ore
management samples were determined of by this method, the relative errors were -4.55%-4.35%, and the measured values
were consistent with the standard value. This method should be used in production practice, and good measurement results
have been achieved.
Keywords：X-ray fluorescence spectrometry; fusion sample preparation; stone coal vanadium ore; major and minor components
柳金良，张鑫，宋茂生. 熔融制样- X 射线荧光光谱法同时测定石煤钒矿中12 种主次成分[J]. 化学分析计量，2019，28(3)：25-28.
LIU J L，ZHANG X，SONG M S. Simultaneous determination of 12 major and minor components in stone coal vanadium ore by X-ray fluorescence spectrometry with fusion sample preparation[J]. Chemical analysis and meterage，2019，28(3)：25-28.