Replication Data for: An Improved Electron Microprobe Method for the Analysis of Halogens in Natural Silicate Glasses

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Replication Data for: An Improved Electron Microprobe Method for the Analysis of Halogens in Natural Silicate Glasses
Flemetakis, Stamatis; Berndt, Jasper; Klemme, Stephan; Genske, Felix; Cadoux, Anita; Louvel, Marion; Rohrbach, Arno, 2021, "Replication Data for: An Improved Electron Microprobe Method for the Analysis of Halogens in Natural Silicate Glasses", https://doi.org/10.35003/ILUU2B, TRR170-DB, V1, UNF:6:C6uJExp1oo5G0S7Hj+iTGA== [fileUNF]
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Description
We present a new analytical method, which allows the simultaneous analysis of fluorine (F), chlorine (Cl), bromine (Br), and iodine (I) in geological samples. To account for interferences of Fe on the spectral lines of F, of Al on Br-lines, and of Ca on I-lines, we prepared four new halogen-free calibration glasses. The new method is used to analyze various glass reference materials and crystal-hosted melt inclusions from the Azores. Our results show that our new method allows reliable and reproducible analyses of all four halogens in silicate glasses. (2020-08-10)
Subject Chemistry; Earth and Environmental Sciences
Keyword Bromine, Electron probe microanalysis, Fluorine, Halogens, Iodine
Related Publication Flemetakis, S, Berndt, J, Klemme, S, Genske, F, Cadoux, A, Louvel, M, and Rohrbach, A (2020) An Improved Electron Microprobe Method for the Analysis of Halogens in Natural Silicate Glasses. Microsc Microanal 26(5), 857–866. doi: 10.1017/S1431927620013495
Notes TRR 170 publication no. 105. Please note a correction has been issued for this article: The affiliation for author Anita Cadoux has been corrected since original publication. DOI: https://doi.org/10.1017/S1431927620024551
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An-improved-electron-microprobe-method-for-the-analysis-of-halogens-in-natural-silicate-glasses.pdf
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Fig. 1. (a) Calibration line for F. Glasses with different Fe contents were used from ~0.4 to ~14 wt% (Table 1). There is an almost linear correlation (R2 = 0.9962) with increasing Fe content. The 95.45% confidence line indicates that the error (2 SD) on the F content because of Fe is relatively small (±40 μg/g) up to ~9 wt% and increases (±80 μg/g) at higher concentrations. (b) Calibration line for Br that quantifies the effect of Al in the analysis signal. Our glasses have an Al2O3 content ranging from ~1 to ~18 wt% (Table 1). The excess Br signal we get from Al also shows a linear relation (R2 = 0.9891) with an increasing amount of Al inside the samples. Based on the 95.45% confidence lines, the error (2 SD) at the excess Br for Al concentrations higher than 12 wt% is ±20 μg/g, while it increases significantly at concentrations less than 2 wt%, probably due to the absence of glasses with very low Al contents. (c) Calibration line for I shows the effect of Ca-interference on the I measurements. The Ca compositional range of our glasses is from 0.4 to ~14 wt% (Table 1). The correlation between the glasses with different Ca contents and the excess I in the signal of the analysis has a linear correlation (R2 = 0.9958). The 95% confidence lines show that the error (2 SD) at the excess I for Ca concentrations from ~5 to ~14 wt% is ±20 μg/g, while it increases at low concentrations (<2 wt%) at 40 μg/g.
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Fig. 2. (a) Fluorine literature data for the glasses VG-A99, VGA-568, VG-2, AC-E, DR-N, GS-N, BCR-2G, and BHVO2-G (Marks et al., 2016; Zhang et al., 2016), compared with F data from the present study. Fluorine concentrations from each study can be found in Tables 2 and 3. The dashed line represents the 1:1 line. Our results are plotted mainly against the data from Zhang et al. (2016), in order to show the good agreement of the individual studies. Glasses VGA-568, VG-A99, and VG-2 show differences that are discussed inside the text and are attributed to glass inhomogeneity. (b) Chlorine literature data for the glasses VG-A99, VGA-568, VG-2, AC-E, DR-N, GS-N, BCR-2G, and BHVO2-G (Marks et al., 2016; Zhang et al., 2016), compared with Cl data from the present study. Chlorine concentrations from each study can be found in Tables 2 and 3. The dashed line represents the 1:1 line. Our results are plotted mainly against the data from Zhang et al. (2016) and show an overall excellent agreement.
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Fig. 3. Fluorine versus Cl data in olivine-hosted melt inclusions from the Azores show good agreement between datasets obtained with different instruments and methods. Particularly, the two datasets obtained on melt inclusions from Pico island span the same Cl–F space. 1Present study, 2Métrich et al. (2014), and 3Rose-Koga et al. (2017). The table with the individual data can be found in Supplementary Table 2.
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Table 1. Major Elements (wt%) Composition and “Apparent” Halogen Contents (μg/g) of Halogen-Free Glasses Used for the Calibration.
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Table 2. Reference Glasses Analyzed in the Present Study and Their F, Cl contents (μg/g).
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Table 3. Fluorine and Cl Contents of Reference Glasses from the Literature Compared With Our Study.
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Table 4. Bromine Contents (μg/g) and Accuracy of Reference Glasses Analyzed in Our Study and in Cadoux et al. (2017).
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