NMR of residual protons in partly deuterated anisotropic materials with phase-alternated decoupling of deuterium spins

A new method is presented for decoupling spins with S = 1 like deuterium in anisotropic media while observing other spins such as residual protons in partly deuterated samples. The carrier frequency of a weak radiofrequency (RF) field is applied near the center of the doublet arising from the quadrupolar interaction of the S = 1 spins. The phase of the RF field is periodically reversed with intervals matching the reciprocal of the magnitude of the quadrupolar splitting. It is shown by theory and experiment that, even when the irradiating field is quite weak, the efficiency of this phase-alternated decoupling scheme is much better than for simple continuous-wave irradiation at the center of the doublet, an established technique which is usually referred to as double quantum decoupling. The phase-alternated experiment makes it possible to decouple large quadrupolar interactions with a weak RF field. A theoretical analysis and numerical simulations are presented to demonstrate the decoupling performance. Proton spectra of partly deuterated dibromobutane in a liquid crystalline solvent have been recorded to illustrate the efficiency of phase-alternated deuterium decoupling.