86 



THE ALUMNI JOURNAL. 



Incompatibility of Sodium Phosphate and the 

 Alkaloids.— Chrisiiaens calls attention to the 

 incompatibility of sodium phosphate (Na^H 

 PO4) with solutions of the alkaloids, being of 

 alkaline reaction, its deportment to the alka- 

 loids would be the same as that of the alkalies 

 themselves. When added to a solution contain- 

 ing an alkaloid, this is slowly deposited in the 

 bottom of the container and is liable to be taken 

 at an entire dose. — V. C. 



Simple or Mixed Ethers of Parffian Series.— 

 Krafft and Roos, of Heidelberg, have patented 

 a new and simple process for preparing these 

 ethers which depends on the reaction between 

 an alcohol of the paraffin series and a mono or 

 di-sulfonic acid of the aromatic series, thus ; 

 ist. CeH.SOaOH-l-CaHsOH^ 



CH^SO^OC.Hj-l-H.O 

 2d. C^H^SO^OC^Hj-l-CHjOH^ 

 C^H.OC^H^-l-CeHsSO^OH 



The phenyl sulfonic acid regenerated can be 

 used over again, it being capable of converting 

 over one hundred times its weight of ethyl 

 alcohol into ether. As is well known, the sul- 

 fonic acid ester may also be produced by action 

 of a sulfo-chlorid or alcohol, thus : 



a. CgH^SOXl-l-C^HsOH^ 

 CeH.-SO.OCaHH-HCl 



b. C6H5S020C.,H5-|-C2H.30H= 

 CeHgSOaOH-l-CaHjOC^H, 



This latter synthesis is better adapted to those 

 alcohols of higher molecular weight. For 

 mixed ethers the mixed corresponding alcohols 

 [i. e., methyl and propyl alcohol) are heated 

 with a sulfonic acid. — V. C. 



Opium Assay.— Ti. B. Dott. Ten Gms. of 

 powdered opium are digested with 25 Cc. water; 

 1.8 Gm. barium chloride, dissolved in about 

 12 Cc. water, is then added. The solution made 

 up to 50 Cc, is well mixed, and after a short 

 time filtered ; 22 Cc. (representing 5 Gms. 

 opium) are mixed with dilute sulphuric acid, in 

 quantity just sufficient to precipitate the barium. 

 About I Cc, is required, and the solution should 

 be warmed to cause the precipitate to subside, 

 and the solution to filter clear. To this filtered 

 solution a little dilute ammonia, about 0.5 Cc, 

 should be added to neutralize the free acid, and 

 the solution concentrated to 6 or 7 Cc. , and al- 

 lowed to cool. One Cc. spirit and i Cc. ether 

 are then added, and next ammonia in slight 

 excess. The ammonia should be added gradu- 

 ally until there is no further precipitation, and 

 a perceptible odor of ammonia remains after 

 well stirring and breaking down any lumps 

 with the stirring rod. After three hours the 



precipitate is collected on conterpoised filters^ 

 and washed. Before filtering, it should be 

 noted that the solution has a faint odor of am- 

 monia; if not, one or two drops of ammonia so- 

 lution should be added. The dried precipitate 

 is washed with benzene or chloroform, dried 



and weighed. It is then titrated with — acid 



10 



until the morphine is neutralized, as indicated 



by the solution reddening litmus paper, i Cc. 



Gm. morphine hydrate. 



acid = .0303 



10 



That is on the usual acceptation that the hy- 

 drate is Cj -Hi,,N03.H.O, although, as I have 

 shown, there is good reason to believe that it 

 has the composition Cj ^Hj ^NOg.gHjO. 



The precipitate given by the barium chloride 

 is much less bulky than that given by the B.P. 

 process with its large quantity of lime, so that 

 it is not difficult to allow for its volume with 

 practical accuracy. The barium chloride not 

 only precipitates the meconic acid but also a 

 large proportion of resinoid and impurities 

 which interfere with the precipitation of mor- 

 phine. The barium is entirely gotten rid of by 

 the sulphuric acid, so that there is no risk of car- 

 bonate or basic salt of barium being present in 

 the morphine precipitate, and so causing error 

 in the volumetric estimation. The ammonia 

 added is just the proper amount required to 

 neutralize free acid and to precipitate the mor- 

 phine from its hydrochloride. It is a great at- 

 vantage that it is not necessary to give a longer 

 time than three hours for the morphine to 

 precipitate. No notice need be taken of a very 

 slight precipitate which forms after the mor- 

 phine has been illtered off, as the precipitate 

 does not consist of morphine, but for the most 

 part of calcium meconate. On comparing this 

 method with that above referred to (which we 

 might call "the proof spirit process"), I ob- 

 tained 1.35 Gm. of morphine hydrate, in 

 both cases, from the 10 Gms. of opium: = 

 13.5 per cent. In another opium, assayed twice 

 by the barium chloride process, I obtained 

 precipitates (after washing with chloroform) 



, ^, " . ,. . . N 



a = 0.59; b = 0.59. 



These neutralized of 



10 



sulphuric acid, 16.9 Cc. and 17 Cc,' indicating 

 .51 Gm. and .515 Gm. morphine, i. e.^ 

 the opium was = 10.2 per cent, morphine. I 

 do not mean to say that the results always come 

 out so closely, but the same may truly be said 

 of the best processes for opium assay. It would 

 save time in the analysis if, instead of drying 

 the precipitate and washing with benzene, the 

 liquid containing the precipitate were washed 

 with ether, by decantation, and the washed 



