27 



METHODS FOB THE ANALYSIS OF MEDICINAL PLANTS AND 



DRUGS. 



Twenty-second Convention, 1905, Bui. 99, Cir. 26. 



The method prescribed by the eighth revision of the United States 

 Pharmacopoeia, page 329, for the assay of gum opium, powdered 

 opium, deodorized opium, and granulated opium, was adopted as a 

 provisional method. 



PROVISIONAL METHOD FOR THE ASSAY OP OPIUM (GuM, POWDERED, DEODORIZED, AND 



GRANULATED. ) 



[Eight Revision, U. S. Pharmacopoeia, page 329.] 



Assay of opium. 



* 



Opium, in any condition, to be valued 10.0 gm 



Ammonia water 3.5 cc 



Alcohol, ether, distilled water, lime water, each a sufficient quantity. 



Introduce the opium (which, if fresh, should be in very small pieces, and if dry, in very 

 fine powder) into an Erlenmeyer flask having a capacity of about 300 cc, add 100 cc of dis- 

 tilled water, stopper the flask, and agitate it every ten minutes (or continuously in a mechan- 

 ical shaker) during three hours. Then pour the contents as evenly as possible upon a 

 wetted filter having a diameter of 12 cm, and, when the liquid has drained off, wash the 

 residue with distilled water, carefully dropped upon the edges of the filter and its contents, 

 until 150 cc of filtrate have been obtained. Then carefully transfer the moist opium back 

 into the flask by means of a spatula, add 50 cc of distilled water, agitate it thoroughly and 

 repeatedly during fifteen minutes, and return the whole to the filter. When the liquid has 

 drained off, wash the residue, as before, until the second filtrate measures 150 cc, and finally 

 collect about 20 cc more of a third filtrate. Evaporate carefully in a tared dish, first, the 

 second filtrate to a small volume, then add the first filtrate, rinsing the vessels with the third 

 filtrate, and continue the evaporation until the residue weighs 14 gm. Rotate the concen- 

 trated solution about in the dish until the rings of extract are redissolved, pour the liquid 

 into a tared Erlenmeyer flask having a capacity of about 100 cc, and rinse the dish with a 

 few drops of water at a time until the entire solution, after the rinsings have been added to 

 the flask, weighs 20 gm. Then add 10 gm (or 12.2 cc) of alcohol, shake the flask well, add 

 25 cc of ether, and repeat the shaking. Now add the ammonia water from a graduated 

 pipette or burette, stopper the flask with a sound cork, shake it thoroughly during ten 

 minutes, and then set it aside in a moderately cool place for at least six hours, or over night. 



Remove the stopper carefully and should any crystals adhere to it brush them into the 

 flask. Place in a small funnel two rapidly acting filters of a diameter of 7 cm, plainly folded 

 one within the other (the triple fold of the inner filter being laid against the single side of the 

 outer filter), wet them well with ether, and decant the ethereal solution as completely as 

 possible upon the inner filter. 



Add 10 cc of ether to the contents of the flask, rotate it, and again decant the ethereal 

 layer upon the inner filter. Repeat this operation with another portion of 10 cc of ether. 

 Then pour the liquid in the flask into the filter in portions in such a way as to transfer the 

 greater portion of the crystals to the filter, and, when the liquid has passed through, transfer 

 the remaining crystals to the filter by washing the flask with several portions of water, using 

 not more than 15 cc in all. Use a feather or rubber-tipped glass rod to remove the crystals 

 that adhere to the flask. Allow the double filter to drain, then apply water to the crystals, 

 drop by drop, until they are practically free from mother liquor, and afterwards wash them, 

 drop by drop, from a pipette, with alcohol previously saturated with powdered morphine. 

 When this has passed through, displace the remaining alcohol by ether, using about 10 cc or 



