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Standardless Quantitative Electron-Excited X-ray Microanalysis by Energy-Dispersive Spectrometry: What Is Its Proper
1Surface and Microanalysis Science Division, National Institute of Standards and Technology, Building 222, Room A113, Gaithersburg, MD 20899
Summary
Quantitative electron beam X-ray microanalysis using energy-dispersive spectrometry (EDS) with standards offers high accuracy. Standardless EDS methods show significantly larger errors, impacting analytical results.
Area of Science:
- Materials Science
- Analytical Chemistry
- Physics
Background:
- Quantitative electron beam X-ray microanalysis using energy-dispersive spectrometry (EDS) with standards and matrix corrections provides high accuracy.
- Standardless EDS methods aim to replace physical standards with calculations based on physical models or fitted data.
Purpose of the Study:
- To evaluate the accuracy of different standardless energy-dispersive spectrometry (EDS) analysis procedures.
- To compare the error distributions of standardless EDS methods against traditional methods using standards.
Main Methods:
- Three standardless EDS procedures were tested: one based on first principles and two commercial fitted standards methods.
- A diverse suite of microanalysis standards, including alloys, glasses, minerals, ceramics, and compounds, were used for error distribution measurements.
Main Results:
- Standardless EDS methods exhibited significantly larger error distributions compared to standard-based methods.
- The first-principles standardless procedure had 95% of analyses within +/-50% relative error.
- Commercial fitted standards procedures resulted in 95% of analyses within +/-25% relative error, while standard-based methods achieved +/-5%.
Conclusions:
- Standardless EDS methods, while convenient, introduce substantial errors in quantitative microanalysis.
- Recommendations are provided for the appropriate use of standardless analysis to mitigate accuracy issues.