The amounts of hydroxyl ions released from hydrous alumina during phosphate adsorption were measured at constant pH values and at different phosphate concentrations using an automatic titrator. The hydroxyl ions released were plotted against phosphate adsorbed and the equations that gave best fit to the data were differentiated. The variation in the differentials (dOH/dP) with increasing phosphate adsorption was consistent with the theory, proposed below, on the type of sites responsible for phosphate adsorption, by synthetic hydrous alumina containing bayerite and pseudoboehmite, at different concentrations.At low phosphate adsorption which corresponded to low phosphorus concentration, adsorption took place mainly by displacing aquo groups (Al-H,O). With increase in phosphorus concentration hydroxo groups (Al-OH) became the predominant sites of adsorption. At still higher concentrations, where phosphate adsorption displacing aquo and hydroxo groups was nearly completed, the hydroxyl bridges linking aluminium atoms (AI-OH-Al, 01 groups) were broken. This created new sites which were responsible for additional adsorption of phosphate at these concentrations.