Antimony in the range up to 2.5 mug/ml in the final solution is determined spectrophotometrically with vanillylfluorone in the presence of poly(vinyl alcohol) in acidic media. The method is compared with that using o-hydroxyhydroquinonephthalein (Qnph). It is simple, rapid and sensitive, without need for heating or solvent extraction, and the apparent molar absorptivity () is 5.0 x 10(4) 1.mole(-1).cm(-1) at 545 nm; for the Qnph method is 2.8 x 10(4) 1.mole(-1).cm(-1) at 520 nm. Tests with an artificial wastewater gave 99-103% recovery.