374 Report of the Department of Chemistry of the 



The nitrate from the above was just neutralized with barium 

 hydroxide. The white amorphous precipitate was filtered, washed 

 in water, alcohol and ether and dried in vacuum over sulphuric 

 acid. It weighed 17 grains. It did not contain inorganic phos- 

 phate. It was analyzed after drying at 105° as above: 



Found: C = 9.19; H = 1.42; P = 11.21; Ba = 47.86 per ct. 



CRYSTALLIZATION OF THE WATER-INSOLUBLE BARIUM SALT. 



The water-insoluble barium salt previously analyzed, 5.75 grams, 

 was dissolved in the minimum quantity of 0.5 per ct. hydrochloric 

 acid and the solution heated to boiling. The solution remained 

 perfectly clear. Alcohol was then added until the solution turned 

 slightly cloudy. On scratching, the substance began to separate 

 in a crystalline or granular form on the sides of the flask. 



After standing over night the substance was filtered, washed in 

 water, alcohol and ether and dried in the air. 



The filtrate was precipitated with alcohol, filtered, washed and 

 dried in vacuum over sulphuric acid. It was again dissolved in 

 a small quantity of 0.5 per ct. hydrochloric acid, heated, alcohol 

 added and allowed to stand as before when a further quantity of 

 the same shaped crystalline or granular product was obtained. This 

 was filtered, washed in water, alcohol and ether and dried in the air. 



This product was a heavy snow-white crystalline or granular 

 powder. Under the microscope it looked homogeneous and consisted 

 of small transparent spherical globules. It was free from chlorides 

 and inorganic phosphate. For analysis it was dried at 105° in vacuum 

 over phosphorus pentoxide. 



Found: C=9.91; 11 = 1.83; P= 14.90; Ba = 34.75; H 2 = 12.48 

 per ct. 



This substance was recrystallized in the same manner when it 

 separated in the same form as before. It was again analyzed after 

 drying as above. 



Found: C = 10.06; H = 2.02; P= 15.30; Ba=33.36; H 2 = 11.73 

 per ct. 



Since this substance separated in characteristic crystalline manner 

 and did not show any appreciable change in composition on recrystal- 

 lization one might believe that it was homogeneous. We have, 

 however, been unable to obtain any other preparation having the 

 same composition. Numerous preparations were made which 

 separated in exactly the same manner and form and so far as appear- 

 ance is concerned they looked identical, but on analysis widely 

 varying results were obtained. 



One product gave the following: 



C = 10.67; H - 2.00; P = 14.46; Ba = 35.02; H 2 = 11.97 per ct. 



Another was prepared and recrystallized three times when it gave 

 the following : 



C = 11.60; H = 1.88; P = 12.48; Ba = 34.37; H 2 = 11.60 per ct. 



