hour, were found to contain only 27.6 per cent. iodine, making the resulting compound represent 76-66 per cent. BiOI, with a large amount of BiONO3.H2O, showing conclusively that large quantities of KI remained undecomposed and were lost in the washings, and that there is nothing "definite" in its composition. The washings, when tested with a solution of AgNO3, gave a copious white, curdy precipitate of AgI.

Several samples were made by various other methods, as by "trituration," etc., but none of these were satisfactory, having various percentages of BiOI, from 88 to 95 per cent, with "uncertain" quantities of BIONO, H2O, differing in no special way from those already spoken of.

Of all the methods so far considered I had found no one that was entirely satisfactory. The method of "precipitation" seemed to be in all respects better than any of the others, yet it was far from being perfect. In experimenting upon this process I found that it should be modified as follows: Dissolve 409 grs. BiONO, H2O in 1 fluid ounce HNO, with the aid of heat, as is stated in Mr. England's formula; then carefully dilute this solution with water as long as BiONO, is not reprecipitated, or, at least, until it has assumed a slight permanent opalescence. Add to this 221 grs. of KI, dissolved in about 16 fluid oz. of cold water, in a large flask or some suitable vessel, agitate thoroughly, and then apply heat, but not to the boiling point, (about 80°-85° C.). The mixture at first assumes a black color, growing gradually brownish, becoming still lighter as it is agitated, and under the influence of moderate heat and violent agitation it is finally changed from a light brown to a brilliant red. The agitation is continued for a few moments longer that the reaction may be completed. The precipitate is washed by decantation, drained upon a plain filter and dried at 100° C. The yield should be about 470 grs. The whole operation is completed in a very short while. No iodine is liberated, and hence the product contains a larger and proper percentage of it, and represents a pure article of BIOI.

Bismuthyl iodide so obtained is of a very bright red color, almost vermilion, and has the additional advantage of being in very fine powder, light and bulky, admirably adapted for use as a dusting powder or dressing, an advantage possessed by none of the other specimens. By analysis I found it to contain 35.8 per cent. of iodine, making 99-44 per cent. BiOI, with only 35 per cent. BiONO.H2O.

. Jour. Pharm

, 1889

The reaction taking place in the above is most likely as follows: (1) BIONO.H2O + 2 HNO, = Bi 3 NO, + 2 H2O.

3

(2) 3 (Bi 3 NO3) + 3 KI = Bil, + 2 (Bi 3 NO3) + 3 KNO3. (3) BiI, + 2 (Bi 3 NO2) + 3 H2O = 3 BiOI + 6 HNO3.

(heated-)

The mode of analysis which was pursued in these experiments, is as follows::

For estimation of Iodine.-Place 0.5 gm. BiOI in a flask with a few pieces of test zinc, cover with water, and mix thoroughly, then add sufficient H2SO, to evolve hydrogen slowly, at the same time decomposing the BiOI. Thus H combines with I to form hydriodic acid, while ZnSO, is formed and Bi is precipitated in black flocculent masses. This reaction is completed in two or three hours. Neutralize the resulting mixture carefully with KHO, add a few drops of solution K, CrO, as an indicator; titrate with one-tenth normal solution of AgNO3 until a red precipitate begins to form. The percentage of iodine is then calculated as by U. S. P. process.

For estimation of Bismuth.-Dissolve 0.5 gm. BiOI in a small quantity of nitric acid, dilute with water, boil until all iodine has been vaporized and all odor of HNO, has disappeared; add to this KHO, until a precipitate is formed which does not redissolve on shaking. Collect on a plain filter, wash well, ignite and weigh as Bi2O3.

MEDICINAL CATECHU.

BY EDWIN STANTON REIDER, PH.G.

From an Inaugural Essay.

The examination and estimations presented in this essay were undertaken with the view of ascertaining the medicinal worth of catechu as it is found in the drug market. Eighteen samples were obtained from various sources and the results gotten from these were considered to be a fair indication of the condition of the drug in general.

Samples 1 to 6 were in powdered state, the remainder were in mass. Nos. 1, 2, 7 and 8 were obtained from Baltimore, Md., direct from the jobbers. Nos. 11, 15 and 16 from the same city, but received through retailers. Nos. 5 and 9 were procured from a wholesale drug-house in New York City. The remaining samples were

. Jour. Pharm

, 1889

all gotten in Philadelphia; Nos. 10 and 14 from retail pharmacies, the remaining eight from prominent wholesale establishments. Concerning No. 17, it might be stated that it is neatly put up in fourounce packages and labelled "Catechu Pallidum."

The impurities which these examinations disclosed consisted mainly of leaves, sticks, pebbles and dirt of various sorts. The possibility of the presence, in the drug markets, of catechu that had been treated with potassium-bichromate for dyers' use-as was pointed out in a recent paper (AMER. JOUR. PHARMACY, Oct., 1888), was the incentive for a thorough search, in each sample, for this dangerous impurity, but its absence was proven in every instance. By reference to the appended table it is seen that the moisture ranges from 7.99 per cent. to 14:47 per cent., the powdered samples containing an average of 11.63 per cent. and those in mass 11.65 per cent.

The average yield of ash was very large, No. 14 giving 19.61 per cent., the largest. This sample consisted principally of sticks, leaves and sand, hardly meriting the name catechu. No. 7 showed the lowest ash percentage, viz., 1.67 per cent. ; four other samples yielded less than 3 per cent. No. 17, when ignited for ash gave off a strong odor of burning nitrogeneous matter, and when a portion of the sample was dissolved in hot water the solution had a decided and strong cheese-like odor.

It was noticeable that those samples giving the highest ash percentage also contained iron in the largest proportions, this being especially true of Nos. 2, 9, 14 and 16, all of which gave evidence of its presence in large amounts. The other samples also contained iron in varying amounts, some, notably No. 18, showing its presence but slightly. Nos. 1 and 2 also had aluminium present in small quantities.

The catechu estimations were made as follows: A 1 per cent. solution (0.5 gm. in 50 cc.) of the catechu, in hot water, after cooling, was shaken up with successive portions of stronger ether, the ethereal layer separated after each treatment; these several ethereal solutions were then mixed together and the ether evaporated. The ethereal residue was again treated with stronger ether to dissolve away the catechin from that portion of the aqueous extract which had remained mixed with the first ethereal solutions. This last solution was again evaporated, the residue being pure catechin. As the table shows, the yield of catechin was quite small, the greatest amount obtained from

Am. Jour. Pharm.
April, 1889.

sample No. 11 being 16.50 per cent. The superiority of this specimen over the average commercial catechu was shown also by its dissolving in hot water almost without insoluble residue and giving a very light colored solution. No. 7, although giving a small proportion of catechin, yielded it in a most attractive crystalline form.

To sum up these results, we find that the catechu generally present in the drug market contains small proportions of catechin and correspondingly large amounts of impurities; almost invariably contains iron, and, as far as these results indicate, none has been found to contain potassium bichromate.

Following is a general synopsis of the results obtained:

Sample. Moisture.

Ash.

Catechin.

Remarks.

10-16 per cent. 3.77 per cent. 3.73 per cent. 1ron, trace: aluminium, trace.

1

2

By GEORGE M. BERINGER, PH. G.

Read at the Pharmaceutical Meeting, March 21st.

A sample of ground flaxseed recently offered showed upon examination the following peculiarities: With iodine, the decoction gave a copious reaction for starch; it yielded to petroleum ether 20-92 per cent. of oil; ash, 3 per cent. On examining the sample microscopically the starch was identified as that of corn.

A sample of pure ground flaxseed gave no reaction for starch, and yielded to petroleum ether 32.97 per cent. of oil; ash, 4.5 per cent. The sample offered was evidently adulterated with corn meal to the extent of about forty per cent., judging from the small yield of oil

and ash.

A sample of corn meal examined yielded to petroleum ether only 2.65 per cent. of oil; ash, 1-2 per cent.

It

The adulteration of ground flaxseed with such material is likely quite common, and may be easily detected by the test for starch. is a well-known fact that, although flaxseed may contain starch while growing, in the fully matured seed the starch is entirely converted into albumen and oil. The writer suggests that the Pharmacopoeia should require flaxseed to give with iodine no reaction for starch. As most flaxseed yields considerably over 30 per cent. of oil, I am also of the opinion that the Pharmacopoeia should require it to yield not less than 30 per cent., instead of 25 per cent., as in the present edition.

OLEATE OF MERCURY.

BY A. P. BROWN, PH. G.

Read at the Pharmaceutical Meeting, March 21.

Several years ago Dr. Wolff read a paper on "Oleates" (see AMERICAN JOURNAL OF PHARMACY, 1881, p. 545), and recommended them to be made by decomposing sodium oleate (white castile soap) with a soluble salt of the desired metal. For instance, to make oleate of zinc, a solution of acetate of zinc is added to a solution of oleate of sodium; a white precipitate will fall which, when washed and dried, is termed powdered oleate of zinc. For making oleate of mercury, a solution of oleate of sodium is added to a solution of bichloride of mercury, the mixture becomes milky and in order to separate the oleate of mercury it is necessary to boil the mixture until the oleate forms a yellow mass, when the remaining liquid is poured off and the oleate washed with water, transferred to an evaporating dish and on a water bath heated until all the water is driven off.

Now, in preparing oleate of mercury according to this process, the continued boiling will decompose the oleate and a black precipitate will also form, and instead of being of a beautiful yellow color, a dark mixture resembling mercurial ointment would be the result, consisting of a mixture of oleate and oxide of mercury.

Having occasion to use considerable quantities of oleate of mercury made by this process, I was anxious to have a nice reliable. preparation for dispensing, and it occurred to me that the process might be improved by adopting the following plan :

Take of white Castile soap, in fine powder, 3viii; bichloride of