100 



The crystals are rod-like, frequently with more or less chisel-like ends and a V-shaped 

 recess extending backward into the crystal. There is a strong tendency to form 

 coarse clusters up to about 15 branches. In open drops tree-like forms are frequent. 

 For each of these reagents dilutions up to 1:1,000 give the reaction and the limit at 



Sodium carbonate This gives a precipitate with cocain like that produced by 

 potassium hydrate, both in the amorphous and crystalline forms. Limit of dilution 

 is 1:1,000. In 1:100 solution the limit is 3 //gr. 



In order to ^determine the usefulness of some of the above tests when other alka- 

 loids are present the palladous chlorid test was made*on test drops to which had been 

 added solutions of one of the following alkaloids, codein sulphate, atropin sulphate, 

 heroin, dionin, acoin powder, cinchonin sulphate, hydroxylamin hydrochlorid, 

 apomorphin hydrochlorate, narcotin, papaverin, brucin, narcein, morphin, thebain, 

 gujasanol, orthoform (new), cinchonidia sulphate, quinidia sulphate, beta-eucain, 

 holocain, caffein, quinin sulphate, strychnin, and tropacocain. In each case the 

 crystals of the cocain compound were obtained and in the case of brucin, gujasanol, 

 caffein, strychnin, and tropacocain, with which the palladous chlorid regularly gives 

 a crystalline precipitate, it was found that when cocain was also present the cocain 

 product was given in addition to that for the other alkaloid, though occasionally with 

 modified form. 



The foregoing serves to give an idea of the scope of the work undertaken, which it 

 is hoped will be carried much further during the coming year. 



COOPERATIVE WORK ON HEADACHE MIXTURES. 

 By W. 0. EMERY. 



After making investigations of various suggested methods for determining the different 

 constituents present in the many headache mixtures containing acetanilid and similar 

 agents, a method was finally devised which proved quite satisfactory to the members 

 of the Division of Drugs, and it was therefore decided to place this method in the 

 hands of as many chemists interested in this line of work as could assist. A circular 

 letter requesting cooperation was sent out, and a gratifying number responded, sig- 

 nifying their willingness to assist, eleven of whom sent in results. All who expressed 

 a desire to cooperate were supplied with a sample of a mixture containing known 

 amounts of acetanilid, sodium bicarbonate, and caffein, with the following instruc- 

 tions, the U. S. Pharmacopoeia, eighth revision, as amended and corrected May 1 and 

 June 1, 1907, being used as a basis for all calculations and reagents unless otherwise 

 specified: 



SEPARATION OF CAFPEIN, ACETANILID, AND SODIUM BICARBONATE. 



Caffein. 



\Yeigh out about 0.3 gram of headache powder on a small (5.5 cm) tared filter, 

 wash with successive small portions of chloroform to the amount of about 30 cc, col- 

 lecting the solvent in a 100 cc Erlenmeyer. Distil off chloroform by means of a small 

 flame until only a few cubic centimeters remain. Add 10 cc of dilute sulphuric acid, 

 then continue the distillation till all the chloroform has gone over, disconnect from con- 

 denser, heat gently, first on wire gauze to complete solution, & finally on a steam or hot- 



<In cases of powder mixtures or tablets containing ground celery seed, much color- 

 ing matter, cinchona alkaloids, laxative or extractive principles other than acetanilid 

 or phenacetin, it is our practice to shake out the latter by means of chloroform from 

 dilute sulphuric acid solution. 



*> In case the preparation contains ground celery seed or certain oily principles, 

 it sometimes happens that the acid solution does not become entirely clear at this 

 point. 



