The processes of generation, management, treatment and disposal of fly ash industrial waste particles, all over the world, were considered as serious issues of solid waste. The subject of this research work was to create and to characterize the Fly ash/Chitosan composites aimed for heavy metal adsorption in polluted waters. Three different types of fly ash waste particles were used, two types supplied from EURONICKEL and one supplied from OSLOMEJ, Macedonia. The surface of the fly ash (FA) particles was modified by treated with nitric acid (HNO3). Several types of composite adsorbents were prepared using the chitosan as a polymer matrix. The characterization of the metallurgical waste particles was performed by XRF, XRD, TGA, SEM and FTIR analysis, while the obtained composites were tested by TGA, SEM and FTIR analysis. It was observed that the structure, morphology, and some other characteristics of FA particles have been significantly changed after treatment with chitosan and it is expected that it will improve their adsorption capacity of heavy metal ions.