X射线荧光光谱分析法熔融制样技术的探讨与应用

Discussion and application of sample preparation by fusion in X-ray fluorescence spectrometry

本文选用三种不同熔融制样方式,研究了熔剂的性质、熔融制样的过程及加热方式等制样条件,探讨了X射线荧光光谱分析法的熔融制样技术。通过脱模剂加入量的试验,证明了在温度、熔融体流动性一致的情况下,挥发性脱模剂碘化铵可不必定量加入。针对铁矿石标准样品的特点,以四硼酸锂为熔剂,通过采用预氧化后高温熔融的制样程序,得到了优化的试验条件。结果表明,铁矿石试样熔融制样时间缩短至100 s/样,使得制样速度与粉末压片速度(90 s/样)相接近,优化条件后制样的相对标准偏差为0.4%～6.2%(n=10)。

Three kinds of sample preparation by fusion methods were introduced in this paper,and the sample preparation conditions by fusion in X-ray fluorescence spectrometry were investigated,such as the properties of flux,the process of sample preparation by fusion and the mode of heating.The addition test of release reagent indicated that,the volatile release reagent（ammonium iodide） was not necessarily added in a quantitative way when temperature and fusant fluidity were uniform.According to the characteristic of iron ore certified reference materials,the optimal experimental conditions were obtained by high temperature fusion after pre-oxidation using lithium tetraborate as flux.The results showed that the fusion time for iron ore sample was shortened to 100 s/sample,which made its sample preparation speed close to that of pressed powder pellet（90 s/sample）.The relative standard deviation（RSD,n=10） of sample preparation after optimization was 0.4 %-6.2 %.