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A simple, precise, sensitive and accurate method was developed for rapid determination of trace quantities of periodate. The method is based on the accelerating effect of periodate on the reaction of bromate and hydrochloric acid in the presence of hydrazine. The decolorization of methyl orange with the reaction products was used to monitor the reaction spectrophotometrically at 525 nm. Periodate could be determined in the concentration ranges of 0.02–1.5 μg/mL. The relative standard deviation for ten replicate determinations of 0.3 μg/mL of periodate was 1.12%. The method was applied to the determination of periodate in water samples and indirect determination of ethylene glycol in gasoline and glycerol in vegetable oil via Malaprade reaction with satisfactory results.