Intense sample heating through high-speed magic-angle spinning (MAS; up to 58 K temperature difference) is demonstrated. The role of probehead and spinner design, as well as that of the temperature of the bearing air on the heating of a rotating sample, is examined. MAS-induced heating can affect the accurate determination of the isotropic value of the chemical shift as well as the principal values, asymmetry and anisotropy parameters of the chemical shift tensor. In some cases, a very large temperature gradient (12 K) within the fast rotating sample was found, which may limit the resolution of high-speed 1H MAS nuclear magnetic resonance (NMR) spectra.

Institute of Macromolecular Chemistry Academy of Sciences of the Czech Republic Prague

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