APPENDIX. 287 



,WT1 



Successive 15 c.c. chloroform, and after separation these were dr 

 off in turn and mixed. The mixed chloroformic solutions were 

 then shaken up with four successive small portions of acidulated 

 water, by which means all the alkaloid was taken out, together 

 with the mother-liquor included in the chloroform magma, and 

 the latter separated out clear. The acid solutions were mixed and 

 made alkaline, and the alkaloids ^gain shaken out with three 

 successive portions of chloroform. The Tatter were drawn off and 

 mixed and the process repeated (usually five or six times) until a 

 point was reached where the alkaloi^al' solution became almost colbui'- 

 less, and a perfectly clear chlorofoi'mic solution was obtained. 



When 



were once more 



extracted with acidulated wateiv the latter solution made alkaline, 

 the alkaloids again taken out with chloroform, the chloroforaiic 

 solution shaken with ammoniated water, and after separation drawn 

 off and evaporated and the residue dried at 100*^ and weighed. The 

 loss of alkaloid by this process is very slight, and there- is no waste 

 of chloroform^ the same portion being employed all the way through 

 for shaking out the alkaloids, a fresh quantity being used only for 

 the final extraction of the ptu'e alkaloid. The process, however, was 



tedious 



hours. 



'llowin 



to shorten materially the time occupied by eadi estimation : 



The chloroform magma is inti'oduced into a separating funnel and 

 shaken vigorously, when, as a rule^ about half the chloroform 

 separates out and can be ran off. To the remaining emulsion 5 c.c. 

 of 90 per cent, alcohol is added and the whole well shaken and then 

 allowed to stand^ when a perfect separation into two layers takes 

 place, the lower layer cx)nsisting of chloroform and alcohol, and the 

 upper layer of a brown alkaline aqueous liquid. The whole of the 

 alkaloid is taken oirt by the chloroforai. The latter is drawn off and 

 added to the portion previously separated and the alkaloid extracted 

 by shaking with three portions of acidulated water. The acid solu- 

 tions are mixed and made alkaline and the alkaloids recovered by 

 means of chlorofonn. This process is once repeated, and the final 

 chloroformic solution, after shaking with ammoniated water, is 

 drawn off and evaporated, and the residue dried at 100'' and weighed. 

 These two modific-ations of the process of estimatioD were tried side 



