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Iron speciation in minerals and glasses probed by \(\hbox{M}_{2/3}\)-edge X-ray Raman scattering spectroscopy

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Abstract

We present a spectroscopic study of the iron \(\hbox{M}_{2/3}\)-edge for several minerals and compounds to reveal information about the oxidation state and the local coordination of iron. We describe a novel approach to probe the iron \(\hbox{M}_{2/3}\)-edge bulk sensitively using X-ray Raman scattering. Significant changes in the onset and shape of the Fe \(\hbox{M}_{2/3}\)-edge were observed on ferrous and ferric model compounds with Fe in octahedral and tetrahedral coordination. Simulation of the spectra is possible using an atomic multiplet code, which potentially allows determination of, e.g., crystal-field parameters in a quantitative manner. A protocol is discussed for determination of the Fe oxidation state in compounds by linear combination of spectra of ferric and ferrous end members. The presented results demonstrate the capabilities of Fe \(\hbox{M}_{2/3}\)-edge spectroscopy by X-ray Raman scattering to extract information on the ratio of trivalent to total iron \(\hbox{Fe}^{3+}/\sum \hbox{Fe}\) and local coordination. As X-ray Raman scattering is performed with hard X-rays, this approach is suitable for in situ experiments at high pressure and temperature. It thus may provide indispensable information on oxidation state, electronic structure and local structure of materials that are important for physical and chemical processes of the deep Earth.

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Acknowledgments

We acknowledge ESRF, APS, SPring-8 and DELTA for providing synchrotron radiation. AN and KM would like to thank BMBF (05K10PEC and 05K13PE2) for financial support. JST and RAG acknowledge the support from NSERC of Canada (MFA, Discover grant). The authors would also like to thank M. Stuff and D. Rhede (GFZ) for the electron microprobe analysis of the AOQ-2 sample and J. Pohlenz for proof reading.

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Author notes

  1. L. Simonelli

    Present address: ALBA Synchrotron Light Facility, CELLS, Barcelona, Spain

Authors and Affiliations

  1. Fakultät Physik/DELTA, Technische Universität Dortmund, 44221, Dortmund, Germany

    A. Nyrow, C. Sternemann, K. Mende & M. Tolan

  2. Section 3.3, Deutsches GeoForschungsZentrum, 14473, Potsdam, Germany

    M. Wilke

  3. PNCSRF, APS Sector 20, Argonne, IL, 60439, USA

    R. A. Gordon

  4. Photon Science, DESY, 22607, Hamburg, Germany

    H. Yavaş

  5. European Synchrotron Radiation Facility, 38043, Grenoble Cedex, France

    L. Simonelli

  6. National Synchrotron Radiation Research Center, Hsinchu, 30076, Taiwan

    N. Hiraoka

  7. Department of Physics, University of Helsinki, P.O. Box 64, 00014, Helsinki, Finland

    Ch. J. Sahle & S. Huotari

  8. Dipartimento di Scienze della Terra, Sapienza Università di Roma, 00185, Rome, Italy

    G. B. Andreozzi

  9. Institut für Geowissenschaften, Universität Frankfurt, Altenhöferallee 1, 60438, Frankfurt, Germany

    A. B. Woodland

  10. Department of Physics and Engineering Physics, University of Saskatchewan, Saskatoon, S7N 5E2, Canada

    J. S. Tse

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  1. A. Nyrow
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  2. C. Sternemann
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  6. H. Yavaş
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  9. Ch. J. Sahle
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Correspondence to A. Nyrow.

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Communicated by J. Hoefs.

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Nyrow, A., Sternemann, C., Wilke, M. et al. Iron speciation in minerals and glasses probed by \(\hbox{M}_{2/3}\)-edge X-ray Raman scattering spectroscopy. Contrib Mineral Petrol 167, 1012 (2014). https://doi.org/10.1007/s00410-014-1012-8

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  • DOI: https://doi.org/10.1007/s00410-014-1012-8

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