A common method for the preparation of hydroxylamine has been to pass sulfur dioxide gas slowly into a cold mixture of sodium nitrite and sodium carbonate in water until the solution is just acid to litmus.1 The hydroxylamine disulfonate ion formed by this process was hydrolyzed by heating the solution, which was then evaporated to dryness and the hydroxylamine extracted as either the sulfate or chloride. The following equations represent the two steps N02-+ 2HS03-+ H+ = H0N(S03)2-+ h2o H0N(S03)2" + 2H20 = HONH3+ + 2SOr + H +
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