This work presents an experimental study investigating the formation and oxidation of particulate matter from the combustion of heavy fuel oil, HFO, droplets. The study includes results from both a falling droplet in a drop tube furnace and a suspended droplet in a heated convective flow. The falling droplets in a heated coflow air with variable temperature path and velocity were combusted and the resulting particles, cenospheres, were collected. To characterize the microstructure of these particles, scanning electron microscopy (SEM), and energy dispersive X-Ray (EDX) analysis were used. The particles were found to have either a porous or a skeleton/membrane morphology. The percentage of particles of either type appears to be related to the thermal history, which was controlled by the heated co-flow velocity. In the suspended droplet experiments, by suspending the droplet on a thermocouple, the temperature inside the droplet was measured while simultaneously imaging the various burning phases. A number of specific phases were identified, from liquid to solid phase combustion are presented and discussed. The droplet ignition temperature was seen to be independent of the droplet size. However, the liquid phase ignition delay time and the droplet lifetime were directly proportional to the initial droplet diameter.