Vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol have been found to chemiluminesce by the action of potassium permanganate in sulphuric or polyphosphoric acid media. Both acid media have been compared and sulphuric acid allows the sensitive determination of 0.15-10.0, 0.010-1.0 and 0.0030-0.30microg mL(-1) of vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol with limits of detection equal to 0.045, 0.0030 and 0.00090microg mL(-1), respectively. Recoveries of vanillin from commercial vanillin products are within the range of 95-109%. Comparison with results from the official method shows differences within the range of 0.5-3.0%. The chemiluminogenic reaction mechanism is also discussed.