The combustion of different fuels gives rise to the formation of small but appreciable amounts of volatile organic compounds (VOCs). They basically result from incomplete combustion and their emissions have negative repercussions on health and on the environment in general. As their measurement is difficult, costly, and very time-consuming, very little is reported on the emissions of VOCs from combustion installations. In this study, various blends of two different coals with several wastes were burned in a pilot-scale fluidized bed combustor and measurements of VOCs at several locations along the combustor height as well as just before the stack were carried out. The results demonstrate that the parameters important for the formation of VOCs are temperature, excess air levels, and the effectiveness of the mixing of air with fuel. Furthermore, it was observed that coal was the principal source of VOCs, but the combustion of volatiles from fuels such as biomass, occurring in the freeboard, was important in reducing the emissions of VOCs to almost zero.