The first combined multiple pulse-magic angle experiment is reported in which both homonuclear dipole interactions and chemical shift anisotropies are removed to resolve chemically shifted fluorines. The sample selected was KEL-F.(AIP)

High-resolution nuclear magnetic resonance spectra of protons in rigid, randomly oriented solids have been measured using combined homonuclear dipolar decoupling (via multiple pulse techniques) and attenuation of chemical shift anisotropies (via magic-angle sample spinning). Under those conditions, isotropic proton chemical shifts were recorded for a variety of chemical species, with individual linewidths varying from about 55 to 110 Hz (1–2 ppm). Residual line broadening was due predominately to (i) magnetic-field instability and inhomogeneity, (ii) unresolved proton–proton spin couplings, (iii) chemical shift dispersion, (iv) residual dipolar broadening, and (v) lifetime broadening under the multiple pulse sequences used. The magnitudes of those effects and the current limits of resolution for this experiment in our spectrometer have been investigated. The compounds studied included organic solids (4, 4′-dimethylbenzophenone, 2, 6-dimethylbenzoic acid, and aspirin), polymers (polystyrene and polymethylmethacrylate), and the vitrain portion of a bituminous coal.

An NMR probe is described which is capable of use in combined multiple pulse–magic angle spinning experiments for removal of homonuclear dipolar broadening and chemical shift anisotropies in randomly oriented samples. Two examples are included to illustrate the utility of the technique.