the greatest care in the addition, breakage could not be avoided. I therefore concluded to try the old method, by oxidizing the phosphorus in a glass retort, with results entirely satisfactory. The following is the process pursued by me, which I can recommend as perfectly safe:

Introduce into a French glass tubulated retort of capacity of 42 parts, 12 parts of water and two parts of phosphorus. Place the retort on a sand bath and introduce through a funnel tube, fixed in the tubulure by means of a cork and reaching half an inch below the level of the liquid, eight parts of nitric acid. Apply gentle heat and watch the operation closely as soon as reaction commences. When the reaction slackens add more nitric acid in portions of about one-fourth part at a time. Should the reaction become violent, small quantities of warm water must be added until it is reduced to its ordinary action, which may be compared to the gentle boiling of water. The formation of frothy bubbles on the surface of the liquid is always the forerunner of violent reaction and should be checked at once. I have found that if it was checked at this stage, a comparatively small amount of water would answer, but if allowed to react violently a much larger quantity of water was necessary. The evaporation of the acid, after the phosphorus is all oxidized, is conducted in a porcelain capsule; towards the end of this process it will froth up, owing to the rapid disengagement of nitric oxide. The dish must therefore have about three times the capacity of the acid when concentrated, and a little distilled water should be kept conveniently near, to add in case there is danger of frothing over. It is scarcely necessary to add that the operation should be conducted under a good furnace hood, or otherwise the beak of the retort should be introduced into a good flue.

Sulphate of Manganese. Wishing to make some of this salt, I adopted the following formula, which gives an abundant yield of the pure salt:

Introduce into an iron crucible a mixture of five parts of peroxide of manganese and three-fourth parts of coarsely powdered charcoal. Cover the crucible and heat to redness until all the charcoal is consumed. Allow the contents of the crucible to cool, place in a porcelain dish and add 6 parts of

sulphuric acid. Evaporate nearly to dryness, return the mass to the crucible and heat to redness. When cool rub to powder, if necessary, and treat twice successively with eight parts of boiling water; mix the liquors, filter and evaporate until a pellicle begins to form, when set aside to crystallize.

If evaporated too far an insoluble sulphate is deposited, (probably in a peculiar state of hydration), hence care must be taken to remove it from the sand-bath as soon as a pellicle begins to form. When a good article of peroxide of manganese is used, this formula will give an abundant yield of perfectly pure sulphate of manganese. Any iron or copper present is destroyed by heating the crude salt to redness.

Ammonio-ferric Alum. In making this salt according to the U. S. Pharm. formula I found that, instead of obtaining crystals of a clear violet tinge, they had a brownish color. I first ascribed it to unskilful manipulation, but on repeated trials met with similar results, sometimes, however, approaching in appearance to the commercial article. As the addition of a small quantity of sulphuric acid to a solution of salt prevents its decomposition, caused by the formation of a basic ferruginous salt, I concluded to try the effect of a little sulphuric acid, and met with perfect success. By the addition of 1 fl. oz. sulphuric acid to 1 gall. liquor ferri tersulphat., I obtained crystals of a beautiful violet tinge and perfect form. These were simply drained thoroughly and immediately bottled. I have been so far unable to obtain the salt perfectly dry without injuring its appearance. The mother liquors will yield another crop of crystals if evaporated gently and filtered. If the solution is not filtered the salt will have a rusty appearance from the decomposition of a portion of the salt. Where large quantities are made it is better to use the mother liquors with a new portion of materials.

Tinct. Chlor. Iron. When the Pharmacopoeia direction is strictly followed in making the solution of sesqui-chloride of iron for this tincture, there is danger of the liquid frothing over towards the completion of the process, unless the capacity of the dish is very much larger than the bulk of its contents. By long-continued heat a portion of the muriatic acid, present in the preparation before the oxidation is completed, is also wasted

and frequently sufficient to cause a basic chloride to be formed, which, when mixed with the alcohol, is deposited, sometimes immediately, sometimes after the lapse of a few weeks. This has happened to me on several occasions and others have had similar experience. For several years I have pursued the following manipulation in its manufacture, and have met with invariably satisfactory results. The materials and relative proportions used are the same as in the officinal process:

Make the solution of proto-chloride of iron according to the officinal directions and filter. Heat it to the boiling point, add the reserved portion of muriatic acid, and take immediately from the sand-bath. Into another vessel (capable of holding one-half more than the solution will measure when completed), pour threefourths of the nitric acid required. Place the vessel in the sand-bath from which the solution of chloride of iron has been removed, and add the latter in small portions as long as effervescence is produced. If effervescence should cease before all the iron salt is oxidized, nitric acid must be added in small portions until the completion of the process. Proceeding in this manner the same result is obtained as required by the Pharmacopoeia, the danger of frothing is avoided 'and a permanent tincture is obtained.

Dilute Hydrocyanic Acid. It is well known that when this acid is not carefully secluded from light it is rapidly decomposed and deposits a black substance (Paracyanogen). Wittstein, in his formula for this acid, recommends the use of alcohol as a preservative, and I wish to state that I have prepared an acid according to this formula which has kept without any apparent change for four months, although freely exposed to the light during that entire period. His formula is as follows:

Dissolve 4 oz. ferrocyanide of potassium in 16 oz. of distilled water, to which add a cold mixture of 3 oz. sulphuric acid and 12 oz. alcohol, sp.gr. 840. Allow the mixture to stand for twentyfour hours, shaking it occasionally. Separate the crystalline deposit by means of a strainer and introduce the clear liquid into a retort, the bottom of which is covered to the depth of one inch with clean quartz sand. Distill off 20 fl. oz. and reduce the distillate to the proper strength by the appropriate tests.

The object of using sand in the retort is to prevent the thumbing which is always a source of great trouble during the latter part of the distillation.

Louisville, Ky.

NOTES ON LIQUOR BISMUTHI.

BY GEORGE F. H. MARKOE.

Much has been written on the preparation of Liquor Bismuthi both in this country and in England, where it was introduced by Mr. Schacht. Mr. R. C. Tichborne was the first to make known the composition of the solution, in an able paper to the London Pharmaceutical Society, in which he proved the bismuth to be present in the form of an ammonio-citrate.

Mr. N. Gray Bartlett, in a paper published in the Jan., 1865, number of the Am. Journal of Pharmacy, gave an excellent working process for the making of citrate of bismuth and ammonia in scales, and also in solution.

The writer has used Mr. Bartlett's process many times, and always with good results, but considers the modifications suggested by Mr. A. E. Ebert, published in the Am. Jour. Pharm., Jan., 1866, of much practical advantage, as it shortens the process, especially the washing of the citrate of bismuth on the filter, which is at best a tedious operation.

The writer has but one new point to suggest, and that is with regard to an improved method of assaying the bismuth solution. Sulphide of ammonium and sulphydric acid are the reagents usually employed in the assay of bismuth solutions and give very good results, but they both possess a most disgusting odor. The writer has found that sulphide of sodium, while it gives excellent results, equal in accuracy to those obtained by the use of the first named reagents, has the advantage of giving a denser and hence a more easily washed precipitate of ter-sulphide of bismuth. It has but little odor and can be used in the shop or laboratory without filling the atmosphere of the room with the smell of sulphuretted hydrogen. The point of saturation is readily determined, and the sulphide of bismuth formed is absolutely insoluble in an excess of the precipitant.

Sulphide of sodium may be prepared by the following formula: Take of solution of soda three parts, and conduct sulphydric acid gas into the solution as long as it is absorbed, and when the saturation is complete add two more parts of solution of soda and keep the sulphide of sodium in well stopped bottles.

With a view to test the value of sulphide of sodium as a reagent a number of assays of commercial sample of liquor bismuthi were made. Both of the samples were of New York make, and are furnished to the trade in pound bottles.

No. 1. A colorless liquid with a sweet taste and the flavor of caraway, leaving an after-taste of metallic character. The specific gravity at 60° was 1.45. Four assays of this solution were made by precipitating the bismuth as ter-sulphide by means of an excess of sulphide of sodium, and the average results of these assays were eight and one-half grains of ter-sulphide of bismuth from each fluid-ounce, equal to seven and seven-tenths grains of teroxide of bismuth, or fifteen and four-tenths grains of ammoniocitrate of bismuth. This solution, then, is just what it purports to be, as stated on the label, which claims that the solution contains sixteen grains; the deficiency of six-tenths of a grain in a fluid-ounce being so small that it may be referred to the loss consequent on the manipulation in making the assay.

No. 2. A colorless liquid, having an alcoholic odor and a specific gravity of 995; it was free from flavor and sugar, having only an alcoholic flavor, and the peculiar metallic after-taste of ammonio-citrate of bismuth. The average result of four assays. was five and six tenths grains of ter-sulphide of bismuth, equal to five and eight-hundreths of grains of ter-oxide of bismuth, or ten and sixteen-hundreths grains of ammonio-citrate of bismuth. The label on the bottle of this liquor bismuth states that each teaspoonful of the solution contained two grains of the ammoniocitrate of bismuth, which would be sixteen grains of the bismuth salt in each fluid-ounce. The quantity found was only 10-16 grains, showing a deficiency of about six grains in each fluid

ounce.

The writer has found the loss of citrate of bismuth in his practice to be about seven per cent., a quantity too small to pay for the time and trouble of regaining by the use of sulphuretted