Analytical Sciences

Fullerene as a Standard Sample for Adjusting the NMR Spectral Resolution in Multiple-Quantum Magic-Angle-Spinning Experiments

Yuichi SHIMOIKEDA,* Hiroaki UTSUMI,* Koji SAITO,** Tadashi SHIMIZU,*** and Toshihito NAKAI*

*JEOL Ltd., 3-1-2 Musashino, Akishima, Tokyo 195-8558, Japan
**Nippon Steel Corporation, Futtsu, Chiba 293-8511, Japan
***National Institute for Material Science, 3-13 Sakura, Tsukuba, Ibaraki 305-0003, Japan

A method using fullerene for adjusting the NMR spectral resolution for multiple quantum magic angle spinning (MQMAS) experiments is proposed. To observe its ¹³C MAS signal, it is not necessary to apply ¹H decoupling, unavailable with single-resonance MQMAS probes. Although ¹³C T₁ of fullerene is rather long, a recycle time of 5 s in shimming yields its signal with sufficiently high sensitivity if setting the appropriate Ernst angles corresponding to magnetic fields. It is demonstrated that so-adjusted high resolution is reflected in the ⁸⁷Rb MQMAS spectra of RbNO₃.

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