This paper presents research on separating and concentrating titanium(IV) from aqueous sulfuric acid solution, using trioctylamine (TOA) as extractant and kerosene as a diluent. We investigated the effects of reaction time, temperature, sulfuric acid concentration, organic/aqueous phase ratio, TOA concentration, and titanium concentration on the removal efficiency of titanium(IV). The results show that it is possible to recover over 99% of titanium(IV) after 15 min reaction time by TOA from the sulfuric acid solution under the optimum operation conditions and the loading capacity of TOA for titanium (IV) is 30 g Ti(IV)/100 g TOA. We expect that results studied would be applicable to separate and concentrate titanium from secondary sources such as red mud produced in the aluminum/alumina industry.