igos.] HALL AND SMITH— COLUMBIUM. 189 



the material from the Haddam locality showed no more evidence 

 of neptunium than did that from South Dakota. 



Ten kilograms of the main bulk of the potassium columbium 

 oxyfluoride were crystallized from strong hydrofluoric acid. Five 

 hundred grams were taken at one time and the mother liquors from 

 the two fractions combined, evaporated one half, and another crop of 

 crystals removed. The mother liquors from these were united and 

 evaporated, the crystals obtained were recrystallized, the mother 

 liquors from the recrystallization combined and evaporated to dryness 

 with sulphuric acid. The oxide obtained from that portion evapo- 

 rated to dryness was 5 grams. The fraction of crystals immediately 

 preceding, 60 grams in weight, was decomposed with sulphuric acid 

 and the oxide obtained from it. The 5 grams of oxide and about one- 

 half of the oxide from the 60 grams of double fluoride were heated 

 in carbon tetrachloride vapors, taking about 2 grams of oxide at a 

 time. The more volatile portion, which should contain the most 

 of the TiCl 4 , was distilled away from the CbOCl 3 . The portions 

 of this liquid were combined, the oxides — 3 grams — obtained 

 from it, and these oxides again heated in CC1 4 . Again only the 

 liquid portion and that of the solid which was carried over mechan- 

 ically was taken. The oxide from this portion was changed to 

 double fluoride. 



Analysis : 



0.567S gram of sample contained 0.2196 gram of oxide and 



0.3390 gram of K.,S0 4 . 

 0.2196 : 0.3390 :: x/2 : 174 x = 225.4. 



Calculated 



K„CbOF 6 H 2 0. Found. 



Oxide 44-52 38. 6 



K 2 S0 4 57-8i 59.7 



Amount of Ti0 2 in the oxide .0594 gram = 29.7 per cent. 



The oxide from the salt taken for analysis was combined with the 

 oxide from the double fluoride not taken for analysis and this with 

 the remaining half of the oxide from the 60 grams of double fluoride 

 mentioned above was mixed with the oxide from all the previous 

 double fluorides which had been tested for titanium and shown its 

 presence in a fair degree. This mixture of oxides was heated in a 

 current of sulphur monochloride, the chloride formed collected 



