Details
| Original language | English |
|---|---|
| Pages (from-to) | 874-882 |
| Number of pages | 9 |
| Journal | Microscopy and Microanalysis |
| Volume | 25 |
| Issue number | 4 |
| Publication status | Published - 1 Aug 2019 |
Abstract
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.
Keywords
- boron, electron probe microanalysis, high-energy background, silicate glass, tourmaline
ASJC Scopus subject areas
- Physics and Astronomy(all)
- Instrumentation
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In: Microscopy and Microanalysis, Vol. 25, No. 4, 01.08.2019, p. 874-882.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Improvement of electron probe microanalysis of boron concentration in silicate glasses
AU - Cheng, Lining
AU - Zhang, Chao
AU - Li, Xiaoyan
AU - Almeev, Renat R.
AU - Yang, Xiaosong
AU - Holtz, Francois
N1 - Funding information: We thank Harald Behrens (LUH) for providing borosi- licate glasses NBS1-0 and NBS1-I, and Michael Wiedenbeck (GFZ at Potsdam) for providing referencedravite.Ingo Horn (LUH) is appreciated for his assis- tance of LA-ICPMS analysis. The stay of Lining Cheng at the Institute of Mineralogy, Leibniz University Hannover, was funded by China Scholarship Council (CSC). We thank Julien M. Allaz, another anonymous reviewer and Editor Daniel Ruscitto for their critical and insightful comments that have greatly improved this paper. Requests for boron-bearing glasses used in this study as microanalytical references can be addressed to the corresponding author. This study was supported partly by Deutsche Forschungsgemeinschaft (DFG) project BE 1720/40.
PY - 2019/8/1
Y1 - 2019/8/1
N2 - 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.
AB - 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.
KW - boron
KW - electron probe microanalysis
KW - high-energy background
KW - silicate glass
KW - tourmaline
UR - http://www.scopus.com/inward/record.url?scp=85068505142&partnerID=8YFLogxK
U2 - 10.15488/11595
DO - 10.15488/11595
M3 - Article
C2 - 31272519
AN - SCOPUS:85068505142
VL - 25
SP - 874
EP - 882
JO - Microscopy and Microanalysis
JF - Microscopy and Microanalysis
SN - 1431-9276
IS - 4
ER -