Preparation of hydroxylamine hydrochloride (hydroxylammonium chloride)
40g of potassium nitrite and 50g of potassium acetate are dissolved in 100ml of ice-cold water and placed in a one-liter filter flask fitted for the introduction of sulfur dioxide through a delivery tube that leads well into the liquid. 750g of crushed ice are added and sulfur dioxide is passed rapidly into the agitated mixture until absorption is complete. (This is indicated by the fact that the odor of the gas persists after shaking.) The temperature must not rise above 0°C and a small amount of ice should still be present in the reaction mixture when saturation is reached at the end of about one half hour. The precipitated potassium hydroxylamine disulfonate is expeditely filtered from the cold liquid, and the moist salt is dissolved in 500ml of 0.5N hydrochloric acid. The solution is heated on the water bath for two hours and then well cooled in ice while 59g of potassium bicarbonate is added in small portions to the liquid in order to neutralize the free acid formed in the hydrolysis. The final solution should be adjusted to a faint acid reaction with hydrochloric acid. Sixty milliliters of alcohol are added to the mixture with good cooling below 10 °C, the precipitated potassium sulfate is filtered off and washed with 75ml of an equivolume mixture of 95% alcohol and water. The washings are combined with the main filtrate, which is now heated to boiling while a solution of 40g of barium chloride 2-hydrate in about 125ml of hot water is added. The solution containing precipitated barium sulfate is digested on the steam bath for one hour and then filtered with the aid of 5-10g of Celite or Filter-Cel. The residue is washed with 50ml of boiling water which is run into the main filtrate. The combined solution is evaporated to dryness, at first over a free flame, and then on the steam bath. The residue is extracted three times with respectively 200-, 100-, and 50ml portions of 95% alcohol, and the alcoholic extract is evaporated (or distilled) to dryness on the water bath. The product remains behind as white crystals. Yield 13-16g.
Inorganic laboratory preparations, by G. G. Schlessinger, 76-77, 1962
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hydroxylamine, Hydroxylammonium chloride, Oxammonium hydrochloride, Hydroxyamine hydrochloride, Hydroxylamine chloride, Hydroxyammonium chloride, Hydroxylamine-1-hydrochloride, CCRIS 4323, CHEMBL542448, HYDROXYLAMINE, HYDROCHLORIDE, NSC26250, EINECS 226-798-2, Hydroxylamine, hydrochloride (1:1), CID443297, NSC 26250, AI3-08779, H0258