Microwave dielectric loss spectroscopy (MDS) has shown remarkable potential as a tool for the observation of changes in elastomer network structure within the interphase region of natural rubber/carbon black composites. During crosslinking (non elemental sulphur system) the dielectric loss progressively increased. However, during ageing at high temperature the dielectric loss decreased. Parallel studies on the unfilled matrix yielded no such variation in dielectric loss. It was therefore concluded that the changes in microwave responses were related to the development of the interphase during curing and its subsequent destruction during ageing. The microwave response was related to the composite mechanical properties as a function of ageing time. The effect of stabiliser was also investigated.