熔融制样-X射线荧光测定锰矿中10种主次成分的条件优化

Condition Optimization of X-ray Fluorescence Spectrometry with Fusion Sample Preparation for Determination of Ten Major and Minor Components in Manganese Ores

中文关键词:  熔融制样  X射线荧光光谱法  锰矿  条件优化

英文关键词:fusion sample preparation  XRF  manganese ores  condition optimization

中文摘要:

      选用Li₂B₄O₇、LiBO₂和LiF （质量比为45∶10∶5）为混合熔剂，NH₄NO₃为氧化剂，LiBr为脱模剂，熔融制作样片，利用岛津1800型X射线荧光光谱分析仪对GBW07261~GBW07266等锰矿标准物质拟合校准曲线，建立了X射线荧光同时测定锰矿中10种主次量组分（SiO₂、Al₂O₃、Fe、MgO、CaO、K₂O、Mn、TiO₂、P、Zn）的快速分析方法.对样品制备以及分析测试过程中的条件（熔剂稀释比例、熔融温度及时间、测定电压电流以及PHA等）进行了优化，在优化条件下，对GBW07263、GBW07265进行重复测定，相对标准偏差（RSD，n=12）低于2%.同时对锰矿标准样品及合成锰矿样品进行分析，结果与参考值一致.

英文摘要:

      A fast and simple approach to directly determine SiO₂、Al₂O₃、Fe、MgO、CaO、K₂O、Mn、TiO₂、P and Zn in manganese ores samples by X-ray fluorescence spectrometer(XRF)was developed. This method used a glass fuse piece technique with Li₂B₄O₇、LiBO₂ and LiF (Mass ratio:45:10:5) as the flux, NH₄NO₃ as the oxidant, LiBr as the stripping agent. Several experimental parameters were optimized, and the analytical figures of merit were evaluated. The components in the certified reference material of GBW07261~GBW07266 were determined by the proposed method. The relative standard deviation (RSD, n=12) was less than 2%. The accuracy test was conducted with synthetic samples. The results were consistent with the certified values.