38 MESSRS. E. FRANKLAND AND B. F, DUPPA'S 



and placed in a copper still immersed in cold water. Over this was gradually poured 

 12600 grms. of a mixture of 3600 grms. alcohol* of 97 per cent., and 9000 grms. 

 concentrated sulphuric acid, taking care that the temperature did not rise high enough 

 to distil off any of the product. The success of the operation depends greatly upon the 

 mode of mixing the alcohol and sulphuric acid, which ought to be performed as follows. 

 The sulphuric acid being placed in a deep stoneware vessel of sufficient capacity, the 

 alcohol is conducted to the bottom of it by means of a piece of narrow glass tube, con- 

 nected by a caoutchouc tube with a convenient reservoir standing at a considerable 

 elevation. The glass tube is used as an agitator during the continuance of the flow 

 of the alcohol. In this way there is obtained, without loss of alcohol, a high tempera- 

 ture which greatly favours the formation of sulphovinic acid. This mixture must be 

 allowed to stand, carefully covered up, for twenty-four hours before use. 



It is also advisable to make the admixture of sulphovinic acid and sodium acetate 

 at least twelve hours before the distillation is commenced. The latter operation can 

 then be performed over a naked fire or gas-flame, and continued till water alone passes 

 over. In this way there was obtained 6000 grms. of an acetic ether absolutely free 

 from alcohol, and which, without previous washing, only needs one rectification from 

 fused and powdered chloride of calcium to fit it for the action of sodium. A determi- 

 nation of its vapour-density gave the number 2-9. Pure acetic ether requires 3-04. 



When acetic ether thus prepared is placed in contact with sodium it becomes hot, 

 and a considerable quantity of gas is evolved, which, after being passed first through 

 alcohol and then through water, bums with a non-luminous flame, and the products of 

 combustion do not produce the slightest turbidity on agitation with baryta-water. In 

 fact the gas is pure hydrogen. When the action is complete, the liquid solidifies on 

 cooling to a mass resembling yellow beeswax. By putting the sodium into the acetic 

 ether as just described, it is difficult to conduct the operation to completion, owing to 

 the liquid gradually assuming such a thick and pasty condition as to prevent the further 

 action of the sodium. We therefore adopted the foUovdng modification, which enabled 

 us to push the reaction almost to its extreme limit. 



A (fig. 1) is a flask containing the acetic ether, and standing in an oil-bath, B. The 

 neck of the flask was closed with a caoutchouc cork, through which passed the beak of 

 the quilled receiver C, containing the sodium cut up into pieces about 1 inch square 

 and ^ inch thick. Into the wide neck of this receiver was inserted an inverted Liebig's 

 condenser, D, which projected sufficiently into the vessel to allow the condensed liquid 

 to drip back upon the sodium. Heat being applied to the oil-bath, the acetic ether 

 soon began to boil, and by its condensation in C and D not only kept the surface of the 

 sodium constantly moist with fresh portions of acetic ether, but also dissolved off the 

 solid sodium-compound as fast as formed. As the operation progressed it was found 

 necessary to raise the temperature of the oil-bath, so as to cause the continuous distil- 

 lation of the remaining acetic ether, which acquired a higher boiling-point as the pro- 



* Methylated spirit may be used for this purpose. 



