The objective of this thesis is to explore the methods of multidimensional NMR that have been developed to observe ultra slow motions in solids. To achieve this goal both the theoretical and experimental aspects of these experiments are discussed and examples are given for both spectral analysis techniques and time domain methods. To perform these experiments a capable NMR spectrometer is required, the essential aspects of this instrument are discussed, along with the circuit diagrams and software for a pulse programmer that was built as part of this project. The 2D spectral methods are used to determine the jump angle and rate in several crystalline solids these include (' CH'3)3 'SeNO'3 - ' d'3, ('CH'3)3 ' TeI' - 'd'6 and ('CH' 3)3'SI' - 'd'6. For each sample the exchange rates are given for several temperatures along with a 2D experimental and theoretical spectrum. The 2D time domain techniques are used to study two glasses, a glucose/water mixture and a propylene carbonate/phosphoric acid mixture. For both of these samples the average jump angle is determined along with the width of the distribution.