A highly selective and sensitive catalytic method for the determination of trace amounts of titanium(IV) was developed. The method is based on the catalytic effect of titanium(IV) on the methylene blue-ascorbic acid redox reaction. The reaction was followed spectrophotometrically by measuring the change in absorbance of methylene blue at 665 nm, 5 minutes after the initiation of the reaction. In this study experimental parameters were optimized and the effect of the presence of various cations and some anions on the determination of titanium(IV) was examined. The calibration graph was linear in the range of 3-25 ng mL -1 of titanium(IV). The relative standard deviation for the determination of 10 and 20 ng mL -1 of titanium(IV) were 2.64% and 1.51%, respectively (n = 8). The detection limit calculated from three times of standard deviation of blank 3S b was 0.6 ng mL -1 . The method was successfully applied to the determination of titanium(IV) in tap water and ore samples.