702 PROCEEDINGS OF THE AMERICAN ACADEMY. 



1. 100 c.c. (1/5) of the solution required 35.88 c.c. KOH (0.9078 N/5) 



2. " " " 35.88 CO. KOH (0.9078 N/5) 



3. " " " 21.74 c.c. AgNOa (N/1; Volhard) 



4. " " " 21.69 c.c. AgNOs (N/1; Volhard) 



A gravimetric analysis of Sample C resulted as follows: 



5. 0.9400 g. substance gave 2.0352 g. BaS04 



6. 1.0806 " " 2.3009 g. BaS04 



7. 1.1917 " " 1.5891 g. AgCl 



8. 1.1813 " " 1.5751 g. AgCl 



Found. gif^^^ 



Sulphur: (1) 29.93, (2) 29.93, (5) 29.75, (6) 29.80 29'.82 



Chlorine: (3) 33.14, (4) 33.07, (7) 32.99, (8) 32.99 32.98 



Preparations of Chlorsulphonic Acid. 



10. Dry hydrochloric acid gas was passed into 150 g. oleum (91.1 

 per cent) for two hours, the flask being kept cool by ice water. After 

 expulsion of the hydrochloric acid, distillation between 149° and 170° 

 (chiefly 152-155°) yielded 101 g. (theory, 113 g.), and the residue, 

 which was practically all sulphuric acid, weighed 72 g. (theory, 73 g.). 

 On treating the 101 g. with 60 g. salt and distillation under diminished 

 pressure, only 1.5 g. were obtained, which, from melting point and action 

 with water, appeared to be unchanged chlorsulphonic acid. 



11. 165 g. oleum (89.3 per cent) were used. The flask was not 

 cooled. The yield of distillate between 135° and 164° was 89 g. (theory, 

 100 g.), and the residue was 97 g. (theory, 96 g.). 



12. 147 g. oleum (89.3 per cent) were treated as in Preparation 11. 

 The product was then distilled in a current of hydrochloric acid, and 

 88 g. (theory, 89 g.) were obtained from 148° to 151°, the residue 

 weighing 82 g. (theory, 86 g.). 



13. 526 g. oleum (93.9 per cent) were saturated with hydrochloric 

 acid as in Preparation 11. Of the total increase in volume, two thirds 

 resulted from passing the gas rapidly for two hours, one third in an 

 additional five hours. On distilling in hydrochloric acid, 528 g. were 

 obtained, boiling chiefly from 150° to 154° (theory, 512 g.). 



14. The oleum contained 86.2 per cent SO3. The method was as 

 in Preparation 11, but weights were not recorded. 



15. 419 g. oleum (88 per cent) were used ; the method was as in 

 Preparation 11. 261 g. product were obtained, the distillation with 

 hydrochloric acid being very slow (theory, 212 g.). 



16. 333 g. oleum (85.3 per cent) were heated on the steam bath and 



