The proposed determination of gold( III) is based on the formation of dicyanoaurate(I) and its extraction into 1,2-dichloroethane as an ion-pair with Methylene Blue. The optimum pH range for the formation of dicyanoaurate(I ) is 2.2 -7.2 under the conditions described. The absorbance of the extract is stable for at least 4 days in a glass-stoppered tube. The apparent molar absorptivity for gold is 1.08x 105 I mol-' cm-' and the Sandell sensitivity for 0.001 absorbance is 1.8X103 µgAu cm-2 at 657 nm. Linear calibration graphs are obtained over the range 2x107-8x106 --M gold(Ill) (0.4-15.8 µgAu in 10 ml); at the 6x106 M gold(Ill) level, the relative standard deviation is 0.2%.