510 PROFESSOR DITTMAR AND MR C. A. FAWSITT ON 



much regret now that this idea did not suggest itself to our minds in the 

 preparative stage of our work. We thought only of the Wohler process ; 

 how we applied it we shall now proceed to explain. 



The raw material which we started with was a particular fraction of wood- 

 spirit, which had been collected for us in the course of an industrial distillation. 

 50 c.c. of this spirit, when subjected to distillation in a fractionating flask, gave 

 the following results : — 



Boiling-point at a given stage of the distillation = f . 



Total volume of distillate obtained at that stage = v c.c. 



t = 67° 



69° 



70° 



72° 



75° 



v= 



20 



30 



40 



50 c.c. 



Two analyses by the iodide-method gave 71*8 per cent, of real CH 4 ; by 

 Kramer and Grodzki's iodoform test we found 5*6 per cent, of acetone. 



Before applying the oxalate process we thought we had better subject our 

 alcohol to some kind of preliminary purification. We accordingly tried to 

 remove the acetonic compounds by means of alkaline bi-sulphite ; but no 

 modification of the method led to satisfactory results. We then gave a trial to 

 the now almost forgotten method of Kane (fixation of the CH 4 by means 

 of a large excess of fused chloride of calcium, removal of what remains volatile 

 by distillation, regeneration of the alcohol from the CaCl 2 -compound by dis- 

 tillation with water). In this case we worked quantitatively, and determined 

 the acetone in the several fractions as iodoform. The result was highly dis- 

 couraging ; a considerable proportion of the methyl-alcohol escaped combina- 

 tion with chloride of calcium, and the part fixed by the reagent included a 

 considerable proportion of acetone. 



After this second failure we decided upon confining ourselves to the use of 

 caustic soda as a preliminary purifier ; this agent was sure to decompose at 

 least the acetate of methyl ; and, if used dry and in quantity, could be 

 expected to destroy at least part of the acetone. In order to ascertain how 

 far the power of the reagent goes in the latter sense, we heated 100 c.c. of the 

 crude spirit with 150 grammes of powdered caustic soda over a water-bath 

 at the " wrong end " of a condenser for some hours, and next distilled over 

 what could be volatilised by immersion of the flask in a boiling water-bath. 

 We obtained 8 c.c. of a distillate smelling strongly of ammonias, and containing 

 4*6 per cent, of its weight of acetone. The residue was then decomposed with 

 water, and distilled over a naked flame. It furnished a distillate which when 

 tested with iodine and caustic soda gave no iodoform. We did not stop to 

 ascertain what had become of the acetone, but at once applied the process to 

 larger quantities of the spirit, with this modification, however, that we used 

 less proportions of caustic soda in order not to lose too much of the CH 4 0, 

 which could not be expected to survive the process in its entirety. Not caring 



