A highly sensitive spectrophotometric method for determination of arsenic, based on the formation of an ion-association complex between arsenoantimonomolybdenum blue and Malachite Green, has been developed. The ion-association complex is soluble in the presence of Triton X-305, so arsenic can be determined directly in aqueous solution. The apparent molar absorptivity for arsenic is 1.13 x 10(5) l.mole(-1).cm(-1) at 640 nm. Beer's law is obeyed for 0-5 mug of arsenic. The lower limit of determination (absorbance = 0.01) is 4 ng ml in the final solution.