Hydroxylamine has been determined by its oxidation to nitrite with a known excess of bromine. Bromine in acidic medium bleaches the dye methyl red. A known excess of bromine when treated with hydroxylamine is reduced to bromide and the unreacted bromine is determined using methyl red. The method obeys Beer's law in the range 0-5 mu g of hydroxylamine in an overall aqueous volume of 25 mL. The relative standard deviation is 2.7% (n=10) at 3 mu g of hydroxylamine. The molar absorptivity is calculated to be 9.8x 10(4) Lmol(-1)cm(-1) with the correlation coefficient of 0.995. The developed method has been applied for the determination of hydroxylamine and its derivatives after hydrolysis in drug formulations. Tile results obtained by the present method compare well with those obtained by the Verma-Gupta's method and with the standard addition of hydroxylamine and recovery studies.