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A Mössbauer-based XANES calibration for hydrous basalt glasses reveals radiation-induced oxidation of Fe

  • Elizabeth Cottrell EMAIL logo , Antonio Lanzirotti , Bjorn Mysen , Suzanne Birner , Katherine A. Kelley , Roman Botcharnikov , Fred A. Davis and Matthew Newville
Published/Copyright: March 31, 2018
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American Mineralogist
From the journal American Mineralogist Volume 103 Issue 4

Abstract

Oxygen fugacity (fo2) exerts first-order control on the geochemical evolution of planetary interiors, and the Fe3+/ΣFe ratios of silicate glasses provide a useful proxy for fO2. Fe K-edge micro-X-ray absorption near-edge structure (XANES) spectroscopy allows researchers to micro-analytically determine the Fe3+/ΣFe ratios of silicate glasses with high precision. In this study we characterize hydrous and anhydrous basalt glass standards with Mössbauer and XANES spectroscopy and show that synchrotron radiation causes progressive changes to the XANES spectra of hydrous glasses as a function of radiation dose (here defined as total photons delivered per square micrometer), water concentration, and initial Fe3+/ΣFe ratio.

We report experiments from eight different radiation dose conditions and show that Fe in hydrous silicate glasses can undergo rapid oxidation upon exposure to radiation. The rate and degree of oxidation correlates with radiation dose and the product of water concentration and ferrous/ferric iron oxide ratio on a molar basis (Φ = XHO0.5·XFeO/XFeO1.5). For example, a basalt glass with 4.9 wt% dissolved H2O and Fe3+/ΣFe = 0.19 from its Mössbauer spectrum may appear to have Fe3+/ΣFe ≥ 0.35 when analyzed over several minutes at a nominal flux density of ~2 × 109 photons/s/μm2. This radiation-induced increase in Fe3+/ΣFe ratio would lead to overestimation of fO2 by about two orders of magnitude, with dramatic consequences for the interpretation of geological processes.

The sample area exposed to radiation shows measureable hydrogen loss, consistent with radiation-induced breaking of O–H bonds, associated H migration and loss, and oxidation of Fe2+. This mechanism is consistent with the observation that anhydrous glasses show no damage under any beam conditions. Cryogenic cooling does not mitigate, but rather accelerates, iron oxidation. The effects of beam damage appear to persist indefinitely.

We detect beam damage at the lowest photon flux densities tested (3 × 106 photons/s/ μm2); however, at flux densities ≤6 × 107 photons/s/µm2, the hydrous glass calibration curve defined by the centroid (derived from XANES spectra) and Fe3+/SFe ratios (derived from Mössbauer spectra) is indistinguishable from the anhydrous calibration curve within the accuracy achievable with Mössbauer spectroscopy. Thus, published Fe3+/ΣFe ratios from hydrous glasses measured at low photon flux densities are likely to be accurate within measurement uncertainty with respect to what would have been measured by Mössbauer spectroscopy.

These new results demonstrate that to obtain accurate Fe3+/ΣFe ratios from hydrous, mafic, silicate glasses, it is first necessary to carefully monitor changes in the XANES spectra as a function of incident dose (e.g., fixed-energy scan). Defocusing and attenuating the beam may prevent significant oxidation of Fe in mafic water-bearing glasses.

Keywords: XANES; Mössbauer; oxygen fugacity; oxidation state; iron; glass; synchrotron radiation; hydrous basalt; Invited Centennial Article

Acknowledgments

With admiration, we thank Catherine McCammon, who graciously provided her raw Mössbauer spectra and laboratory notes to E.C. We thank Tim Gooding for laboratory support at Smithsonian. E.C. gratefully acknowledges support from NSF EAR 1347248, NSF EAR 1426717, and NSF OCE 1433212. S.K.B. was further supported by OCE-1434199/OCE-1620276. K.K. gratefully acknowledges support from NSF EAR 1347330 and NSF OCE 1433182. We are grateful for support from Smithsonian’s Scholarly Studies program. F.D. also acknowledges support from a National Museum of Natural History Peter Buck Fellowship. We are grateful for support for X26A from Department of Energy (DOE) GeoSciences DE-FG02-92ER14244. The DOE Office of Science supported use of the NSLS under contract no. DE-AC02- 98CH10886. We acknowledge the support of GeoSoilEnviroCARS (Sector 13), which is supported by the National Science Foundation—Earth Sciences (EAR-1128799), and the Department of Energy, Geosciences (DE-FG02-94ER14466). This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under contract no. DE-AC02-06CH11357. We thank editorial handling by Sasa Bajt and Keith Putirka as well as two anonymous reviewers for constructive comments that improved the submission.

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Received: 2017-8-4
Accepted: 2018-1-9
Published Online: 2018-3-31
Published in Print: 2018-4-25

© 2018 Walter de Gruyter GmbH, Berlin/Boston

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https://doi.org/10.2138/am-2018-6268
Keywords for this article
XANES; Mössbauer; oxygen fugacity; oxidation state; iron; glass; synchrotron radiation; hydrous basalt; Invited Centennial Article

Articles in the same Issue

  2. A Mössbauer-based XANES calibration for hydrous basalt glasses reveals radiation-induced oxidation of Fe
  4. Craters of the Moon National Monument basalts as unshocked compositional and weathering analogs for martian rocks and meteorites
  6. Characterizing the source of potentially asbestos-bearing commercial vermiculite insulation using in situ IR spectroscopy
  8. Nanocrystalline apatites: The fundamental role of water
  10. New petrological, geochemical, and geochronological perspectives on andesite-dacite magma genesis at Ruapehu volcano, New Zealand
  12. Combined Fe-Mg chemical and isotopic zoning in olivine constraining magma mixing-to-eruption timescales for the continental arc volcano Irazú (Costa Rica) and Cr diffusion in olivine
  14. Feldspar Raman shift and application as a magmatic thermobarometer
  16. Partial melting of ultramafic granulites from Dronning Maud Land, Antarctica: Constraints from melt inclusions and thermodynamic modeling
  18. Cesium adsorption isotherm on swelling high-charged micas from aqueous solutions: Effect of temperature
  20. Ni-serpentine nanoflakes in the garnierite ore from Campello Monti (Strona Valley, Italy): Népouite with some pecoraite outlines and the processing of Ni-containing ore bodies
  22. Presentation of the 2017 Roebling Medal of the Mineralogical Society of America to Edward Stolper
  24. Acceptance of the 2017 Roebling Medal of the Mineralogical Society of America
  26. Presentation of the Mineralogical Society of America Award for 2017 to Dustin Trail
  28. Acceptance of the Mineralogical Society of America Award for 2017
  30. Presentation of the Dana Medal of the Mineralogical Society of America for 2017 to Thomas W. Sisson
  32. Acceptance of the Dana Medal of the Mineralogical Society of America for 2017
  34. Presentation of the Distinguished Public Service Award of the Mineralogical Society of America for 2017 to David W. Mogk
  36. Acceptance of the Distinguished Public Service Award of the Mineralogical Society of America for 2017
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