Power plant ash was used to synthesize new materials by hydrothermal treatment and ultrasonic activation in an alkaline medium (5 M NaOH) under moderate experimental conditions. The obtained materials were characterized by a variety of techniques (SEM/EDS, INAA, XRD, FTIR, BET). Preliminary investigation of the Ba, Cd, Cr, Cs, Eu and U removal efficiency was performed by batch experiments using radiotracers and spectroscopic techniques as well as desorption studies. The results indicated that the new materials are very efficient in removing the above mentioned metals from aqueous solutions and can be considered as potential low-cost sorbents in environmental technology.