CONTRIBUTION TO STUDY OF HYDROXYLAMINE. — MACKAY. 325 



nitrite to two parts of sodium carbonate," which would give 

 approximately the same proportions as Divers and Haga, which 

 correspond to the equation 

 2N"aN03 + Na.CO, + iSO^ + H^O = 2HOX(S03Na)2 +00^. 



The method of procedure was as follows : — 



500 grams of commercial crystallized sodium carbonate and 

 237 grams of commercial 8odiu?n nitrite were dissolved in 

 800cc. of warm water, and the solution, contained in a glass 

 cylinder about 10 cm. by 30 cm. in size, placed in a freezing mixture 

 of snow and salt. When the temperature fell to — 5° C, sulphur 

 dioxide was passed into the solution from a siphon, tlie delivery 

 tube acting as a stirrer by being attached to a swivel gear fast- 

 ened near the circumference of a wooden wheel kept in motion 

 by means of a small air engine. When the flow of sulphur 

 dioxide was so regulated that the temperature did not rise above 

 — 3°, sulphonation took from 6 to 8 hours. When the solution 

 thus became neutralized, it was poured into a large flask, a few 

 drops of sulphuric acid added, and tlie whole heated to between 

 90 and 95 degrees in a large water bath until the hydrolysis of 

 the sodium oxyamidosulphonate was about complete, the process 

 requiring about 50 hours. 



The solution was then almost neutralized with sodium car- 

 bonate, cooled to O^ C , evaporated, cooled again to — 8°, and a 

 saturated solution of tertiary sodium phosphate added, when 

 the comparatively insoluble hydroxylamine phosphate would 

 separate out. 



Contrary to the experience of Divers and Haga, on adding 

 the few drops of sulphuric acid to the sulphonated solution to 

 start hydrolysis, no marked rise of temperature took place. 



The following variations in treatment were tried without 

 marked improvement in the yield : 



The addition of more water to the solution before starting 

 hydrolysis ; 



The addition of a larger quantity of acid to start hydrolysis ; 



