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A magnesium vanadate spinel crystal, ideally MgV 2 O 4 , synthesized at 1 bar, 1200 °C and equilibrated under FMQ + 1.3 log f O2  condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter diffraction (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies of T(Mg 0.966 ◻ 0.034 ) and M(V 3+  0.711 V 4+  0.109 Mg 0.180 ), respectively, along with the presence of 0.053 apfu Mg at an interstitial octahedral site (16c). Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (≤3 μm) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscopy (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (~9%) of periclase reflections, which eliminated the interstitial Mg, yielding a structural formula for spinel TMgM(V 3+  1.368 V 4+  0.316 Mg 0.316 )O 4 . This study provides insight into possible origins of refined interstitial cations reported in the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

Investigation of synthetic Mg 1.3 V 1.7 O 4 spinel with MgO inclusions: Case study of a spinel with an apparently occupied interstitial site