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

  • 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.

     

    Abstract: 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.

     

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