In this study the applicability of Carbon-13 NMR and XPS to the detection of chemical changes in a solid composite rocket propellant was studied. Storage at elevated temperatures was used to simulate the propellant ageing process. In the XPS analysis, changes in the sources for the N(1s) and Cl(2p) photopeaks were investigated. The propellant loses "organic" nitrogen as it ages. Changes in the amount of Cl⁻ present are in doubt due to instrumental considerations. Carbon-13 NMR analysis showed that with increasing age of a sample there is a corresponding loss of vinylic groups from the binder. This loss of vinylic character is preferential in the order pendant>>cis>trans. Due to the long scan times involved this method is of limited utility for ageing analysis. / Master of Science