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Ordering of Fe 3+  and Fe 2+  cations between octahedral and tetrahedral sites in synthetic members of the magnetite-ulvöspinel (Fe 3 O 4 -Fe 2 TiO 4 ) solid-solution series was determined using Fe L 2,3 -edge X-ray magnetic circular dichroism (XMCD) coupled with electron microprobe and chemical analysis, Ti L 2,3 -edge and Fe K-edge X-ray absorption spectroscopy (XAS), and unit-cell parameters. Microprobe analyses, cell edges, and chemical FeO determinations showed that bulk compositions were stoichiometric magnetite-ulvöspinel solid solutions. XMCD showed that the surface was sensitive to redox conditions, and samples required re-equilibration with solid-solid buffers. Detailed site-occupancy analysis gave Fe 2+ /Fe 3+  XMCD-intensity ratios close to stoichiometric values.

Fe site occupancy in magnetite-ulvöspinel solid solutions: A new approach using X-ray magnetic circular dichroism