215 



Sulphur as Sulphuric Acid. 



The residue was extracted with water and an aliquot part of the 

 filtrate was treated with barium chloride; 1.69 per cent of the total sul- 

 phur was found. 



Sulphur as Sulphates. 



An aliquot part of the filtrate from the black residue was saponi- 

 fied with sodium hydroxide and total sulphuric acid determined as 

 barium sulphate. Deducting the sulphuric acid found without saponifi- 

 cation treatment, 0.99 per cent of the original sulphur' was found as 

 sulphates, presumably ethyl sulphuric acid and ethyl sulphate. 



Sulphur as Sulphonic Acids and Sulphonates. 

 The filtrate from the barium sulphate obtained in the determina- 

 tion of sulphur as sulphates was evaporated to dryness with potassium 

 nitrate and barium hydroxide, and the residue after ignition, was 

 treated with dilute nitric acid, filtered and weighed as barium sulphate, 

 showing 1.02 per cent of the original sulphur. 



Sulphur in the Insoluble Carbonaceous Residue. 

 The extracted black residue was fused with potassium nitrate and 

 barium hydroxide and the resulting barium sulphate was weighed. It 

 corresponded to 0.12 per cent of the original sulphur. 



Conclusions. 

 From the following results it appears that the formation of ether 



ceases because of the disappearance of the sulphuric acid from the 



generating flask. 



Sulphur was found in the following forms and proportions, referred! 



to their total as 100 per cent. 



Sulphur dioxide escaping from the receiver during dis- 

 tillation 0.96 per cent. 



Sulphur dioxide and sulphites in ether distillate 1 . 03 



Sulphuric acid and sulphates in ether distillate 89 . 42 



Sulphuric acid in ether distillate 46 . 54 



Ethyl sulphuric acid in distillate 8.49 



Ethyl sulphate in ether distillate 34.39 



