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High-resolution ¹⁷O MAS NMR spectroscopy of forsterite (-Mg₂SiO₄), wadsleyite (ß-Mg₂SiO₄), and ringwoodite (-Mg₂SiO₄)

¹ Department of Earth Sciences, University of Cambridge, Downing Street, Cambridge CB2 3EQ, U.K.
² Research School of Earth Sciences, Australian National University, Canberra ACT 0200, Australia
³ Bruker BioSpin GmbH, Am Silberstreifen, 76287 Rheinstetten, Germany
⁴ Department of Chemistry, University of Exeter, Stocker Road, Exeter EX4 4QD, U.K.

Correspondence: ^* E-mail: s.wimperis{at}ex.ac.uk

The high sensitivity of the satellite-transition (ST) MAS NMR technique was exploited to obtain high-resolution ¹⁷O MAS NMR spectra of the three polymorphs of Mg₂SiO₄: forsterite (-Mg₂SiO₄), wadsleyite (ß-Mg₂SiO₄), and ringwoodite (-Mg₂SiO₄). High NMR sensitivity was important in this application because ¹⁷O-enriched, Fe-free materials are required for ¹⁷O NMR and high-pressure syntheses of the dense ß and polymorphs result in a only a few milligrams of these solids. In all, eight distinct O species were identified and assigned: three in forsterite, four in wadsleyite, and one in ringwoodite, in agreement with the number of O sites in their crystal structures. The isotropic chemical shifts extracted are in excellent agreement with a previously published correlation with Si-O bond length. However, unexpectedly large quadrupolar coupling constants were found for the non-bridging O species in the dense polymorphs wadsleyite and ringwoodite.

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