基本参数法X-射线荧光光谱同时分析镍、钴和铁基合金

Simultaneous analysis of nickel,cobalt and iron base alloys using X-ray fluorescence spectrometry with the fundamental parameter method

用基本参数法分析了镍、钴和铁基合金,对每种元素在整个含量范围内用单一校准进行了测定,并获得了满意的结果。研究显示,本方法可以采用多通道光谱仪对主次元素进行分析测定。例如,对镍元素来说,在质量分数0%到100%的浓度范围内,准确度达到质量分数0.14%。我们还发现,在铬的分析中,三级激发很显著,对整体强度的贡献率达到2.4%。通过将三级激发考虑进理论强度计算,方法的准确度可由质量分数0.14%提高到0.10%。对灵敏度进行了最小二乘拟合法校准,研究显示二次拟合多项式用单一校准曲线在整个浓度范围内都能给出很好的结果。在多通道光谱仪中,当通道不再适合谱线重叠时,理论强度重叠校正法是有效的手段。

The method for analysis of nickel, cobalt, and iron base alloys by using the fundamental parametermethod, covering the entire concentration range with a single calibration for each element was evaluated. The results obtained were satisfactory and demonstrated that the method can be applied to the analysis of both major and trace elements with a multi-channel spectrometer. For example,0. 14 （w/%） of accuracy was obtained for nickel within a concentration range of 0 to 100（w/%）. We found that tertiary excitation is significant in the analysis of chromium by contributing up to 2.4 % of the total intensity; the accuracy was improved from 0. 14（w/%） to 0. 10（w/%） by incorporating tertiary excitation in the computation of theoretical intensities. The least squares fitting method for sensitivity calibration was studied; the method with a quadratic fit polynomial pinned to a fixed point gave the best result, covering a range from trace level to 100% with a single calibration line. The theoretical intensity overlapping correction method is effective when channels for overlapping lines are not available in a multi-channel spectrometer.