SO2 removal from coal-fired power plant flue gases can be done by dry, semi-dry or wet desulfurization processes, using limestone or lime containing products as sorbents. In a Brazilian coal power plant there is a dry desulfurization unit to capture SO2 with hydrated lime from the combustion gases. A part of the flying ashes produced is mixed with the bottom coal ashes and the spent sulphated product generated after SO2 capture. This residual solid blend is then buried in a non-productive area, from which coal was already extracted and is studied in this work. According to the authors experience in development and characterization of adsorbents for low temperature dry desulfurization processes and in Thermogravimetric Analysis, this paper shows and discusses a method which was developed to characterize qualitative and quantitatively the chemical and mineral composition of this waste by using Thermogravimetry coupled with mass spectrometry (TG/MS), X-ray fluorescence (XRF) and X-ray diffraction (XRD), to preview new potential industrial applications for this waste.