THE ALUMNI JOURNAL. 



219 



sulphuric acid required distillation in a 

 current of steam for one-half hour until 

 all of the phenol was driven over into the 

 receiver. To o i Gm. of phenol from 85 

 to 150 C. c of bromine solution were ad- 

 ded and the mixture allowed to stand for 

 one-half hour, to this was added a treshly 

 prepared solution of 1.25 Gm. of potas- 

 sium iodide in 30 C. c. of water, the flask 

 securely stoppered and allowed to stand 

 12 hours, when it was titrated with the 

 sodium hyposulphite in order to estimate 

 the amount of liberated iodine. 



The same rationale is applied in the 

 examination of disinfecting powders 

 (containing phenol) in which about 0.5 

 Gm. of the powder is placed in a retort 

 with some water and 50 C. c. ot concen- 

 trated hydrochloric acid. The mixture 

 is heated to boiling and a current of steam 

 passed through the retort until all phenol 

 has passed over. The rest of the opera- 

 tion is already given. 



ESTIMATION OF TOTAL ALKALOIDS. 



By C. C. KELLER. 

 IN CINCHONA BARK. 



The author recommends the following meth- 

 od, which can be completed in a few hours, 

 and which furnishes the alkaloids in as pure a 

 condition as they can be obtained by any 

 other process: 12 grms. of finely powdered dry 

 Cinchona bark, contained in a dry flask of 200 

 c. c. capacity, are digesteii with 90 grms. of 

 ether and 30 grms. of chloroform, and frequent- 

 ly agitated during five minutes; 10 c. c. of 10 

 per cent, ammonia are then added, and the 

 mixture is well shaken. The shaking is con- 

 tinued at intervals for half an hour, when 10 

 c. c. of water (12-15 c. c. in the case of calisaya 

 barks') are added, and the skaking continued 

 until the liquid has become clear. 100 grms. 

 of the chloroform-ether extract, after standing 

 for I or 2 hours to allow the separation of 

 water and powdered bark, are carefully poured 

 into a separating funnel and extracted with 30, 

 20 and then 10 c. c. of i per cent, hydrochloric 

 acid. The acid solution is then collected in a 

 separating funnel, made strongly alkaline with 



ammonia and again extracted three times with 

 a mixture containing in all 10 grms. of chloro- 

 form and 90 grms. of ether. After filtering the 

 solutions of the alkaloids into a tared flask, 

 through a small filter wetted with ether, the 

 chloroform and ether are distilled off", and the 

 residue dried at 80° to 90° and weighed. The 

 weight of the residue corresponds to 10 grms. of 

 Cinchona bark. — Schweiz, Wochenschr . Chem. 

 Pharm. 1S93, jj, 4^9. 



IN COCAO LEAVES. 



Twelve grms. of the powdered cacao leaves 

 are treated in a 250 c. c. flask with 120 grms. of 

 ether. After 15 minutes 10 c. c. of 10 per cent, 

 ammonia are added, and the mixture well shak- 

 en. Precipitation is eff"ected half an hour later 

 by the addition of 20 c c. of water and con- 

 tinued, violent agitation. 100 grms. of the dark 

 green etherial solution are then poured off", and 

 after standing some time to clarify, extracted 

 with 50 c. c. and afterwards with 25 c. c. of 0.5 

 per cent, hydrochloric acid. The acid solution 

 filtered if necessary is made alkaline with am- 

 monia and extracted twice with 40 c. c. of ether. 

 The residue, on distilling off in a tared flask 

 represents the amount of alkaloid in 10 grms. 

 of cocao leaves. The alkaloid is thus obtain- 

 ed as a colorless varnish, which crystallizes af- 

 ter standing some time. 



IN NUX VOMICA SEEDS. 



Twelve grms. of powdered nux vomica seeds 

 are mixed with 80 grms. of ether and 40 grms. 

 of chloroform in a dry flask of 200 c. c. capaci- 

 ty. After half an hour, 10 c. c. of 10 per cent, 

 ammonia are added and vigorously shaken at 

 intervals during an hour. 15 to 20 c. c. of water 

 are then added in 2 to 3 portions to precipitate 

 the drug. When the solution becomes clear 

 after continued shaking, 100 c. c. are poured 

 off and extracted in a separating funnel, first 50 

 and then with 25 c. c. of 0.5 per cent, hydro- 

 chloric acid. The acid solution is then extract 

 ed three times with a mixture of 30 grms. of 

 chloroform and 10 grms. of ether. The united 

 extracts are evaporated in a tared flask, and 

 the residue, which retains chloroform, is repeat- 

 edly treated with 5 c. c. of ether, which is then 

 boiled off, until this residue is obtained in the 

 form of a white crystalline powder. The weight 

 of the residue then represents the amount of 

 alkaloids in 10 grms. of the seeds. — Schzueiz, 

 Wochenschr. Chem. Pharni. — Jour. Soc. Chem. 

 Ind. 



