The effect of hydrothermal treatment of the gel or xerogel of titanium phosphate (TiP) sample on the surface properties was studied using the EDS and FTIR ATR methods. The results show that the hydrothermal treatment of initial titanium phosphate decreases the amount of physically adsorbed water but increases the surface concentration of phosphate groups. Supplementary measurements of electrokinetic properties of modified and hydrothermally modified titanium phosphate samples confirmed an increase of the concentration of acidic groups on the TiP surface. The adsorption affinity of titanium phosphate towards cadmium ions was discussed. It was found that at a low initial concentration of cadmium ions adsorption affinity increases as a result of hydrothermal treatment of TiP gel.