A quick anion-exchange reaction, suitable for the determination of sulphide, has been found to occur on stirring a suspension of lead iodate (solubility product, K(s0) = 1.2 x 10(-13)) with sulphide solution at pH 5-8. After removal of the precipitates of lead iodate and lead sulphide (K(s0) = 3.4 x 10(-28)), the iodate released can be determined by its reaction with acidified iodide to give tri-iodide which is either titrated with thiosulphate or measured spectrophotometrically as its blue complex with starch. Chloride, bromide, iodide, fluoride, oxalate, sulphate, thiocyanate and phosphate do not interfere. Thiosulphate, sulphite, nitrite and thiols do not give an anion-exchange reaction but do interfere in the redox reaction of iodate with acidified iodide. However, this is avoided if they are first oxidized with bromine (the liberated iodate remains unaffected before iodometry.