PATROS-A new MAS exchange method using sideband separation: application to Poly(n-butylmethacrylate)

The tr-ODESSA method (Reichert et al., J. Magn. Reson. 125, 245 (1997)), which is a 1D MAS experiment designed to monitor spin exchange involving both equivalent and inequivalent sites, is extended to situations where the spectrum consists of several spinning side band (ssb) manifolds with small chemical shift anisotropies. To increase the spectral resolution in such situations, the tr-ODESSA sequence is combined with that of PASS to a single experiment, which we term PATROS. In this hybrid experiment, magnetization transfer is monitored by the tr-ODESSA part, while the increase in resolution is provided by the separation of the ssb according to their order, during the PASS part. We demonstrate the feasibility of the method on a standard solid dimethylsulfone (DMS) sample and then apply it to monitor separately the ultraslow motions of the main- and side-chains in the polymer poly(n-butylmethacrylate). Theoretical expressions for the ssb intensities in PATROS experiments are derived and the merits and limitations of the method are discussed. Copyright 2000 Academic Press.