Hostname: page-component-cd9895bd7-hc48f Total loading time: 0 Render date: 2024-12-25T17:00:51.543Z Has data issue: false hasContentIssue false

Improvement of Electron Probe Microanalysis of Boron Concentration in Silicate Glasses

Published online by Cambridge University Press:  18 June 2019

Lining Cheng
Affiliation:
State Key Laboratory of Earthquake Dynamics, Institute of Geology, China Earthquake Administration, 100029 Beijing, China Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, 30167 Hannover, Germany
Chao Zhang*
Affiliation:
Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, 30167 Hannover, Germany State Key Laboratory of Continental Dynamics, Department of Geology, Northwest University, 710069 Xi'an, China
Xiaoyan Li
Affiliation:
Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, 30167 Hannover, Germany State Key Laboratory of Continental Dynamics, Department of Geology, Northwest University, 710069 Xi'an, China
Renat R. Almeev
Affiliation:
Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, 30167 Hannover, Germany
Xiaosong Yang
Affiliation:
State Key Laboratory of Earthquake Dynamics, Institute of Geology, China Earthquake Administration, 100029 Beijing, China
Francois Holtz
Affiliation:
Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, 30167 Hannover, Germany
*
*Author for correspondence: Chao Zhang, E-mail: [email protected]
Get access

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 B 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 B, 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.

Type
Materials Applications
Copyright
Copyright © Microscopy Society of America 2019 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Allaz, JM, Williams, ML, Jercinovic, MJ, Goemann, K & Donovan, J (2019). Multipoint background analysis: Gaining precision and accuracy in microprobe trace element analysis. Microsc Microanal 25(1), 3046.Google Scholar
Analytical Methods Committee (1987). Recommendations for the definition, estimation and use of the detection limit. Analyst 112(2), 199204.Google Scholar
Bastin, G & Heijligers, H (1992). Present and future of light element analysis with electron beam instruments. Microbeam Anal 1(2), 6173.Google Scholar
Bastin, GF & Heijligers, HJM (2000). Quantitative electron probe microanalysis of boron. J Solid State Chem 154(1), 177187.Google Scholar
Bauer, U, Behrens, H, Reinsch, S, Morin, E & Stebbins, J (2017). Structural investigation of hydrous sodium borosilicate glasses. J Non-Cryst Solids 465, 3948.Google Scholar
Berndt, J, Liebske, C, Holtz, F, Freise, M, Nowak, M, Ziegenbein, D, Hurkuck, W & Koepke, J (2002). A combined rapid-quench and H2-membrane setup for internally heated pressure vessels: Description and application for water solubility in basaltic melts. Am Mineral 87(11–12), 17171726.Google Scholar
Demers, H, Horny, P, Gauvin, R & Lifshin, E (2002). WinX-Ray: A new montecarlo program for the simulation of X-ray and charging materials. Microsc Microanal 8(S02), 14981499.Google Scholar
Dingwell, DB, Pichavant, M & Holtz, F (1996). Experimental studies of boron in granitic melts. Rev Mineral Geochem 33(1), 330385.Google Scholar
Donovan, JJ, Lowers, HA & Rusk, BG (2011). Improved electron probe microanalysis of trace elements in quartz. Am Mineral 96(2–3), 274282.Google Scholar
Dyar, MD, Wiedenbeck, M, Robertson, D, Cross, LR, Delaney, JS, Ferguson, K, Francis, CA, Grew, ES, Guidotti, CV & Hervig, RL (2001). Reference minerals for the microanalysis of light elements. Geostand Newslett 25(2–3), 441463.Google Scholar
Fialin, M, Rémy, H, André, JM, Chauvineau, JP, Rousseaux, F, Ravet, MF, Decanini, D & Cambril, E (1996). Extending the possibilities of soft X-ray spectrometry through the etching of layered synthetic microstructure monochromators. X-Ray Spectrom 25(2), 6065.Google Scholar
Fournelle, J, Donovan, J, Kim, S & Perepezko, J (2000).Analysis of boron by EPMA: Correction for dual Mo and Si interferences for phases in the Mo-B-Si system, Institute of Physics Conference Series, London, pp. 425426.Google Scholar
Guillong, M, Meier, DL, Allan, MM, Heinrich, CA & Yardley, BW (2008). Appendix A6: SILLS: A MATLAB-based program for the reduction of laser ablation ICP-MS data of homogeneous materials and inclusions. Mineral Assoc Canada Short Course 40, 328333.Google Scholar
Holtz, F, Dingwell, DB & Behrens, H (1993). Effects of F, B2O3 and P2O5 on the solubility of water in haplogranite melts compared to natural silicate melts. Contrib Mineral Petrol 113(4), 492501.Google Scholar
Horn, I, von Blanckenburg, F, Schoenberg, R, Steinhoefel, G & Markl, G (2006). In situ iron isotope ratio determination using UV-femtosecond laser ablation with application to hydrothermal ore formation processes. Geochim Cosmochim Acta 70(14), 36773688.Google Scholar
Jochum, KP, Dingwell, DB, Rocholl, A, Stoll, B, Hofmann, AW, Becker, S, Besmehn, A, Bessette, D, Dietze, H-J, Dulski, P, Erzinger, J, Hellebrand, E, Hoppe, P, Horn, I, Janssens, K, Jenner, GA, Klein, M, McDonough, WF, Maetz, M, Mezger, K, Müker, C, Nikogosian, IK, Pickhardt, C, Raczek, I, Rhede, D, Seufert, HM, Simakin, SG, Sobolev, AV, Spettel, B, Straub, S, Vincze, L, Wallianos, A, Weckwerth, G, Weyer, S, Wolf, D & Zimmer, M (2000). The preparation and preliminary characterisation of eight geological MPI-DING reference glasses for in-situ microanalysis. Geostand Newslett 24(1), 87133.Google Scholar
Jochum, KP, Weis, U, Stoll, B, Kuzmin, D, Yang, Q, Raczek, I, Jacob, DE, Stracke, A, Birbaum, K, Frick, DA, Günther, D & Enzweiler, J (2011). Determination of reference values for NIST SRM 610–617 glasses following ISO guidelines. Geostand Geoanal Res 35(4), 397429.Google Scholar
Kobayashi, H, Toda, K, Kohno, H, Arai, T & Wilson, R (1995). The study of some peculiar phenomena in ultra-soft X-ray measurements using synthetic multilayer crystals. Adv X-Ray Anal 38, 307312.Google Scholar
London, D (1987). Internal differentiation of rare-element pegmatites: Effects of boron, phosphorus, and fluorine. Geochim Cosmochim Acta 51(3), 403420.Google Scholar
London, D, Morgan, GB & Wolf, MB (1996). Boron in granitic rocks and their contact aureoles. Rev Mineral Geochem 33(1), 299330.Google Scholar
McGee, JJ & Anovitz, LM (1996). Electron probe microanalysis of geologic materials for boron. Rev Mineral 33, 770788.Google Scholar
McGee, JJ, Slack, JF & Herrington, CR (1991).Boron analysis by electron microprobe using MoB4C layered synthetic crystals. Am Mineral 76, 681684.Google Scholar
Meier, DC, Davis, JM & Vicenzi, EP (2011). An examination of kernite (Na2B4O6(OH)2·3H2O) using X-ray and electron spectroscopies: Quantitative microanalysis of a hydrated low-Z mineral. Microsc Microanal 17(5), 718727.Google Scholar
Morgan, GB VI (2015). Practical aspects of the electron probe analysis of boron in silicates using a LSM device with large 2d. Microsc Microanal 21, 1141.Google Scholar
Morgan, GB VI & London, D (1996). Optimizing the electron microprobe analysis of hydrous alkali aluminosilicate glasses. Am Mineral 81, 11761185.Google Scholar
Pichavant, M (1981). An experimental study of the effect of boron on a water saturated haplogranite at 1 Kbarvapour pressure. Contrib Mineral Petrol 76(4), 430439.Google Scholar
Schmidt, BC (2004). Effect of boron on the water speciation in (alumino) silicate melts and glasses. Geochim Cosmochim Acta 68(24), 50135025.Google Scholar
Tiepolo, M, Zanetti, A & Vannucci, R (2005). Determination of lithium, beryllium and boron at trace levels by laser ablation-inductively coupled plasma-sector field mass spectrometry. Geostand Geoanal Res 29(2), 211224.Google Scholar
Wenzel, JT & Sanders, DM (1982). Sodium and boron vaporisation from a boric oxide and a borosilicate glass melt. Phys Chem Glasses 23(2), 4752.Google Scholar
Zhang, C, Koepke, J, Albrecht, M, Horn, I & Holtz, F (2017).Apatite in the dike-gabbro transition zone of mid-ocean ridge: Evidence for brine assimilation by axial melt lens. Am Mineral 102(3), 558570.Google Scholar
Zhang, C, Koepke, J, Wang, L-X, Wolff, PE, Wilke, S, Stechern, A, Almeev, R & Holtz, F (2016). A practical method for accurate measurement of trace level fluorine in Mg- and Fe-bearing minerals and glasses using electron probe microanalysis. Geostand Geoanal Res 40(3), 351363.Google Scholar