Economie Preparation of Hydroxylamine 

 Sulphate. 



by 



Edward Divers, IYI.D., F.R.S., Prof. 



and 



Tamemasa Haga, F.C.S., Rigakuhakushi, late Asst. Prof. 



College of Science, Imperial University. 



In 1887 Raschig made known that hydroxyJamine can be got 

 from a nitrite by sulphonation followed by hydrolysis, and took out 

 patents for its manufacture in this way. As to what extent these 

 patents may have since been worked, and with what success, we have 

 no information ; but we cannot believe that this process has been 

 advantageously carried out without great modification of the directions 

 given. The one we are about to describe is very productive and 

 economical for the preparation of hydroxylamine sulphate, a non- 

 deliquescent salt, readily forming large crystals, and soluble in three- 

 quarters of its weight of water at '20°. 



Commercial sodium nitrite of 95 per cent, purity does not contain 

 more than one per cent, of objectionable matters, such as chloride and 

 nitrate, and is, therefore, pure enough. A concentrated solution of 

 this salt (2 mol.) and of sodium carbonate (1 mol.) pretty closely 

 adjusted in their proportions, is treated with sulphur dioxide till just 

 acid, while it is kept well agitated at 2-3° below zero by immersion in 

 ice and brine. At this temperature, the conversion of the nitrite into 

 oximidosulphonate is apparently perfect. Gently warmed with ;i few 

 drops of sulphuric acid the oximidosulphonate rapidly hydrolyses, 



