Newbury DE
Surface and Microanalysis Science Division, National Institute of Standards and Technology, Building 222, Room A113, Gaithersburg, MD 20899
Microsc Microanal. 1998 Nov;4(6):585-597. doi: 10.1017/s1431927698980564.
: Electron beam X-ray microanalysis with semiconductor energy-dispersive spectrometry (EDS) performed with standards and calculated matrix corrections can yield quantitative results with a distribution such that 95% of analyses fall within +/-5% relative for major and minor constituents. Standardless methods substitute calculations for the standard intensities, based either on physical models of X-ray generation and propagation (first principles) or on mathematical fits to remotely measured standards (fitted standards). Error distributions have been measured for three different standardless analysis procedures with a suite of microanalysis standards including metal alloys, glasses, minerals, ceramics, and stoichiometric compounds. For the first-principles standardless procedure, the error distribution placed 95% of analyses within +/-50% relative, whereas for two commercial fitted standards procedures, the error distributions placed 95% of analyses within +/-25% relative. The implication of these error distributions for the accuracy of analytical results is considered, and recommendations for the use of standardless analysis are given.
采用标准样品并进行计算基体校正的半导体能量色散光谱法（EDS）进行电子束X射线微分析，对于主要和次要成分，可得出定量结果，其分布情况为95%的分析结果相对误差在±5%以内。无标样方法用计算代替标准强度，计算要么基于X射线产生和传播的物理模型（第一原理），要么基于对远程测量标准样品的数学拟合（拟合标准样品）。使用一套包括金属合金、玻璃、矿物、陶瓷和化学计量化合物在内的微分析标准样品，对三种不同的无标样分析程序测量了误差分布。对于第一原理无标样程序，误差分布使95%的分析结果相对误差在±50%以内，而对于两种商业拟合标准样品程序，误差分布使95%的分析结果相对误差在±25%以内。考虑了这些误差分布对分析结果准确性的影响，并给出了无标样分析使用的建议。
