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Quantification of Fe2+/Fe3+ by Electron Microprobe Analysis – New Developments

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Abstract

The measurement of the soft FeLα and FeLβ X-ray emission spectra by electron microprobe (flank method) allows the determination of the iron oxidation state in minerals if our new method for self-absorption correction is applied. It can be shown that the FeLβ/FeLα ratios obtained with the flank method correlate with Mössbauer quadrupole splitting and crystallographic data. This can be explained by the successive distortion of the iron coordination polyhedra with cation substitution. Thus, the electron microprobe data unexpectedly reveal details of the electrostatic field at the crystallographic site. Although the resolution with respect to hyperfine parameters is lower compared to other methods, the Fe2+/Fe3+ determination by electron microprobe bears several advantages: (i) the small sample amount needed, (ii) the small sampling volume ≤1 μm3, (iii) the simultaneous in situ Fe2+/Fe3+ determination and quantitative chemical analysis, (iv) the easy routine sample preparation, (v) the ready availability of an electron microprobe in comparison to a synchrotron.

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Authors and Affiliations

  1. Institut für Mineralogie, Johann Wolfgang Goethe-Universität, Senckenberganlage 28, D-60054, Frankfurt am Main, Germany

    H. E. Höfer

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  1. H. E. Höfer
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Höfer, H.E. Quantification of Fe2+/Fe3+ by Electron Microprobe Analysis – New Developments. Hyperfine Interactions 144, 239–248 (2002). https://doi.org/10.1023/A:1025461907725

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