Microcoils and microsamples in solid-state NMR.

Abstract

Recent reports on microcoils are reviewed. The first part of the review includes a discussion of how the geometries of the sample and coil affect the NMR signal intensity. In addition to derivation of the well-known result that the signal intensity increases as the coil size decreases, the prediction that dilution of a small sample with magnetically inert matter leads to better sensitivity if a tiny coil is not available is given. The second part of the review focuses on the issues specific to solid-state NMR. They include realization of magic-angle spinning (MAS) using a microcoil and harnessing of such strong pulses that are feasible only with a microcoil. Two strategies for microcoil MAS, the piggyback method and magic-angle coil spinning (MACS), are reviewed. In addition, MAS of flat, disk-shaped samples is discussed in the context of solid-state NMR of small-volume samples. Strong RF irradiation, which has been exploited in wide-line spectral excitation, multiple-quantum MAS (MQMAS), and dipolar decoupling experiments, has been accompanied by new challenges regarding the Bloch-Siegert effect, the minimum time resolution of the spectrometer, and the time scale of pulse transient effects. For a possible solution to the latter problem, recent reports on active compensation of pulse transients are described.