Improvement of Electron Probe Microanalysis of Boron Concentration in Silicate Glasses

The determination of low boron concentrations in silicate glasses by electron probe microanalysis (EPMA) remains a significant challenge. The internal interferences from the diffraction crystal, i.e. the Mo-B4C large d-spacing layered synthetic microstructure crystal, can be thoroughly diminished by...

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Bibliographic Details
Published in:Microscopy and microanalysis 2019-08, Vol.25 (4), p.874-882
Main Authors: Cheng, Lining, Zhang, Chao, Li, Xiaoyan, Almeev, Renat R., Yang, Xiaosong, Holtz, Francois
Format: Article
Language:English
Subjects:
Boron
Boron carbide
Boron oxides
Electron probe
Electron probe microanalysis
Electron probes
Manganese
Mass spectrometry
Materials Applications
Monte Carlo simulation
Pulse amplitude
Regression analysis
Scientific imaging
Studies
X-rays
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Summary:The determination of low boron concentrations in silicate glasses by electron probe microanalysis (EPMA) remains a significant challenge. The internal interferences from the diffraction crystal, i.e. the Mo-B4C large d-spacing layered synthetic microstructure crystal, can be thoroughly diminished by using an optimized differential mode of pulse height analysis (PHA). Although potential high-order spectral interferences from Ca, Fe, and Mn on the BKα peak can be significantly reduced by using an optimized differential mode of PHA, a quantitative calibration of the interferences is required to obtain accurate boron concentrations in silicate glasses that contain these elements. Furthermore, the first-order spectral interference from ClL-lines is so strong that they hinder reliable EPMA of boron concentrations in Cl-bearing silicate glasses. Our tests also indicate that, due to the strongly curved background shape on the high-energy side of BKα, an exponential regression is better than linear regression for estimating the on-peak background intensity based on measured off-peak background intensities. We propose that an optimal analytical setting for low boron concentrations in silicate glasses (≥0.2 wt% B2O3) would best involve a proper boron-rich glass standard, a low accelerating voltage, a high beam current, a large beam size, and a differential mode of PHA.
ISSN:1431-9276
1435-8115
DOI:10.1017/S1431927619014612