The present study investigates the heavy metal content of coal fly ash (FA) samples coming from three different sampling points (secondary cyclone, cooler and filter) of a pilot plant combustion facility. The combustion experiments were carried out in a 0.1 MW Circulated Fluidized Bed (CFB) boiler using South African coal, with the addition of limestone for sulfur capture. FA was tested for the presence of selected heavy metals using inductively coupled plasma optical emission spectrometry (ICP-OES); batch leaching tests were conducted as well. The samples were also characterized in terms of their microstructure, chemical and mineralogical composition, total surface area and particle size distribution. Most of the studied metals (Cd, Cr, Cu, Ni, Mn, Zn) showed enrichment in the fine, filter FA particles, while Pb was mostly concentrated in the cooler sample. Regarding leaching characteristics of the examined samples, Cr was found to occur in considerable amounts. Although the use of CFB technology for the combustion of solid fuels steadily gets bigger worldwide, only a very limited number of studies have environmentally assessed CFB-coal FAs to date. Thus, the current study aims to contribute toward building a more integrated knowledge on the environmental impact of this abundant power production by-product.