Jour. Pharm , 1899 QUANTITATIVE ANALYSIS. Atomic Weights.-Ag 107.66, Br 79°76, C 11'97, Cl 35'37, H 1'o, K 39'03, N 14'01, Na 23°0, o 15'96, S 31'98. A-(1) Give an outline of the gravimetric analysis of magnesium sulphate for magnesium oxide, sulphur trioxide and water of crystallization, mentioning the chemical formulas for the precipitates produced and for the substances weighed at the end. (2) Outline the calculations by which you would compute the percentage amount of each constituent found. B—(1) Describe the gravimetric estimation of sodium hypophosphite which you made during this term. (2) Write equations for the reactions involved. (3) How many molecules of sodium hypophosphite are indicated by one molecule of the substance from whose weight the result was calculated? C-(1) Show upon your paper the means which you take to find how much N absolute acetic acid I c.c. of KOH, V. S. will neutralize. (2) 5'986 grammes I of a sample of acetic acid requires 36 c.c. of KOH, V. S. to neutralize it. N Explain why each c.c. of the V. S. used corresponds to 1 per cent. of absolute acetic acid. (3) How many grammes of absolute acid are present in one litre of the preceding sample, if the specific gravity of the liquid is 1048? (4) How many cubic centimetres of NKOH, V. S. will be needed to neutralize I I kilogramme of acetic acid containing 36 per cent. of the absolute acid? (5) How many grammes of absolute acetic acid will this same volume of кон, N I V. S. neutralize? (6) A sample of acetic acid has a specific gravity of 1048 and contains 36 per cent. of absolute acetic acid, how many cubic centimetres of the sample will be needed to neutralize 20 c.c. of N KOH, V. S.? I D-Give the successive steps in the volumetric estimation of potassium bitarN trate by means of I of oxalic acid, V. S., using phenolphtalein as indicator. E-(1) How many grammes of pure Na,S,O,5H2O are used to make one litre V. S.? (2) Explain why this quantity is used. (3) What indicator is employed with this V. S.? (4) Tell how the indicator behaves. (5) Name the four official substances which you estimated with this V. S. during the term. (6) Tell how each was prepared for titration. (7) Name an official substance in the estimation of which by residual titration you employed this V. S. (8) Name the other reagents employed in this same estimation. F-A dry sample of potassium bromide contains potassium chloride. 0'500 gramme of the sample requires 43 c.c. of AgNO3, V. S. for complete precipi N tation, what per cent. of potassium chloride is present? Jour. Pharm May, 1899 G-Give an outline of the official method of assaying opium, telling the uses of the materials, the substance weighed at the end of the process and showing the calculation of the result into percentage of the drug. H-Describe the official method of estimating nitrites. (2) Explain the reactions involved in the estimation of spirit of nitrous ether. (3) Outline the calculations used in finding the percentage amount of the important constitu ent of this substance. MINUTES OF THE PHARMACEUTICAL MEETING. PHILADELPHIA, April 11, 1899. The regular monthly Pharmaceutical Meeting was held in the Museum of the College, with David H. Ross in the chair. There being no corrections, the minutes of the previous meeting were allowed to stand as published. The presentation of papers next occupied the attention of the meeting, the first one being a short communication on "Syrup of Hydriodic Acid," by Edwin H. Wells, of Boston, which was read by Prof. F. G. Ryan. It was as follows: "Much trouble with syrup of hydriodic acid has been experienced from the fact that, as ordinarily prepared, it is quite liable to become colored. "This color has sometimes, doubtless, been due to liberation of iodine, but in the writer's experience, this is not always true, by any means. "In most cases it seems to result from the action of the acid on impurities (coloring matter and ultramarine) contained in the sugar or on the sugar itself; the same difficulty being met with in other acid syrups, such as syrup calcium lactophosphate. "Syrup hydriodic acid prepared from pure materials by the U.S.P. process, but using a light syrup (650 grammes to make 1 litre) made from pure white rock candy crystals, has been kept without change for months in partly filled bottles exposed to light and with occasional opening. 66 Heat, however, causes the syrup to acquire color, and it should not, therefore, be kept in a warm place. "When heavy syrup is employed, a white crystalline deposit sometimes occurs which does not appear when a thin syrup is used, but allowance must be made for the difference in percentage of acid by weight in the latter case. "It seems to be mostly a question of purity of ingredients and syrup hydriodic acid carefully prepared from pure materials is perfectly colorless and limpid, and a permanent and satisfactory preparation." In discussing this subject, Prof. Ryan thought that the most important statements of the author had been covered by Mr. F. W. Haussmann in a paper which appeared in the March issue of this JOURNAL, although he thought that every one would admit that the author's views were well taken. Under the heading "Notes on Materia Medica," Prof. C. B. Lowe presented some criticisms on the 1890 U. S. Pharmacopoeia. The author's remarks were confined to the official vegetable drugs and included suggestions for the more accurate description of some of these drugs, the dismissal of others on the ground of their being little used, and the admission of species which have here Jour. Pharm , 1899 tofore not been recognized in giving the botanical origin of certain vegetable drugs. Professor Ryan did not wholly accord with the author's remarks concerning the dismissal of Apocynum from the Pharmacopoeia, and said that while the drug may be used very little in some localities, it is used to a considerable extent in Ohio and Indiana and some other States, and he, therefore, thought that a very broad view of the subject should be taken when discussing questions pertaining to the use of the drugs of the Pharmacopœia. Prof. Joseph P. Remington was the next speaker and read a paper on "Syrupus Pruni Virginianæ (Acetous)" (see page 209). Samples of the syrup and of the fluid acetract of wild cherry accompanied the paper. Mr. Haussmann wished to know the object in directing 150 c.c. of glycerin in the official formula for this syrup, as he found it to keep very well with a less quantity of glycerin. Then, remarking on the quality of the wild cherry bark of the market, he said that he had experienced considerable difficulty in obtaining the drug of uniform quality and believed that the trouble was due to the bark having been collected in the spring and summer rather than in the fall of the year. Prof. Remington in reply said that the use of glycerin had been two-fold-to hold the tannin in solution and to prevent precipitation. He believed that many of the fluid extracts and syrups of the Pharmacopoeia would be improved by placing the glycerin in the receiving vessel rather than by adding it to the menstruum as now directed. The speaker then referred to the experiments of Professor Procter, in 1856, with the fluid extract of wild cherry and said that this preparation had always given more trouble than any of the other preparations of its class. He, therefore, suggested adding the glycerin to the bottle receiving the percolate, rather than to the menstruum, as a means of improving the fluid extract. Prof. F. X. Moerk, having made assays of the dilute acetic acid infusion and of the aqueous infusion directed by the Pharmacopoeia for the syrup of wild cherry, found that the percentage of hydrocyanic acid was about parallel in the two cases, or, if anything, slightly in favor of the acetic infusion, thus showing that the acetic acid had had no injurious effect. F. W. Haussmann read a paper incorporating an improved formula for "Syrupus Rhei," which will be published in a subsequent issue of this JOURNAL. Referring to the formula proposed by the author and to his suggestion to filter the mixture of fluid extract and water before dissolving the sugar in it, Mr. Geo. M. Beringer wished to know whether he had experienced any difficulty in filtering the mixture. In reply, Mr. Haussmann said that he had had no trouble with the official fluid extract, but that the same could not be said of the non-official product. Mr. F. W. E. Stedem related an experience of his, which likewise showed that there is considerable variation in some, at least, of the fluid extracts on the market. These remarks brought up the question of making infusions, syrups, etc., from fluid extracts. Professor Remington did not favor this practice, and to illustrate his view said that while fresh fluid extract of wild cherry contains the desired amount of hydrocyanic acid, an old fluid extract does not contain any of the acid, or very little, and hence a syrup made from such a fluid extract does not possess the value that it otherwise would. Mr. Beringer, while holding in part the same view, said that the practice of making other preparations from fluid extracts was very extensive. He said that syrup of tolu was made almost universally from the liquid tolu. To illustrate further, he said that a few years ago he started putting upon the market a line of fluid extracts without giving formulas for making syrups, etc. The demand for the formulas was so great, that in the end he was obliged to attach new labels, giving the desired formulas. A note on "Tinctura Opii Deodorata cum Camphora," by Thos. S. Wiegand, was as follows: "The tonic effect of opium upon some individuals is as well known as its remedial effect upon the ordinary sufferer. And it is also true, in many instances, that paregoric is not injurious or annoying to persons who cannot take opium in any other form. In view of this fact, the following formula for an improved paregoric is presented: "Macerate the opium two days in an ounce of the ether in a close vessel and then percolate with ether until the percolate is nearly colorless, and a few drops evaporated leave no opium odor; evaporate the percolate to 1⁄2 fluid ounce, add to 1 pint of water and expose it to a gentle heat until all ethereal odor is removed; then dissolve in an ounce of alcohol: I drachm of benzoic acid and I drachm of oil of anise and 40 grains of camphor, to this add 12 fluid ounces of alcohol, mix with the aqueous solution of opium and then add alcohol sufficient to make 2 pints-permit it to stand twenty-four hours, with frequent shaking and filter." A number of interesting specimens were exhibited, as follows: A sample of a new coca base termed by Dr. Schaefer, chemist of the New York Quinine and Chemical Works," cocainidine." Mr. P. Samuel Stout, a student of the College, directed attention to quite a novelty in the way of a clothes-brush. The wood from which the brush was made was sawed from the trunk of a tree which is said to have stood in an ancient forest adjacent to what is now the northern limit of Chicago. This ancient forest is supposed to have been swept into an inland lake, which formerly occupied the present site of Chicago, by a powerful wind storm, and the lake having been filled by driftwood, sand, silt, etc., during the succeeding ages, the remains of the aforesaid forest were completely buried or hermetically sealed. There is evidence that this forest belonged to the vegetation which appeared soon after the glacial period, and so it is estimated that the wood from which the brush was made is 7,000 years old. The brush is the property of the Hon. Joseph M. Gazzam, of this city, and the wood from which it was made was collected by Mr. Ossian Guthrie, the eminent Chicago geologist. Among the other specimens presented were several cocoanuts still in the partly green condition and attached to the branch on which they grew, which were grown in Jamaica, and were received from the India Refining Company, of this city. Mr. H. N. Rittenhouse presented some licorice root, grown in California, which was said to be quite rich in glycyrrhizin. Attention was directed to the flower of a calla, which showed a rather unusual development in that it possessed a double spathe. On motion, the meeting adjourned. FLORENCE YAPLE, Secretary pro tem. HYDRASTINE HEXIODIDE, AND ASSAY OF HYDRASTIS CANADENSIS BY MEANS OF STANDARD IODINE FOR HYDRASTINE AND OF STANDARD POTASSIUM IODIDE FOR BERBERINE. By H. M. GORDIN AND A. B. PRESCOTT. In the work of Research Committee D., Section II, Revision and Publication of the Pharmacopoeia of the United States. When a solution of iodine in potassium iodine is added to a solution of a salt of hydrastine a dense precipitate falls out, of a color varying from light brown to very dark brown. In this order of mixing the alkaloidal solution with the iodine solution, a mixture of different periodides seems to be formed, no matter whether the addition of iodine is stopped while the alkaloid is yet in excess or carried till the iodine is in excess. Even in the first case, that is, when the addition of iodine is stopped long before all the alkaloid is precipitated, the body formed only approaches a triiodide in composition, but does not correspond to a triiodide exactly. As will be seen from the accompanying analysis, the total iodine of the periodide formed under these circumstances agrees quite well with the theoretical amount required by hydrastine triiodide, but the additive iodine is considerably below the amount required by that body. It will be noticed that there is a decided difference in this respect between hydrastine, on the one hand, and strychnine, brucine and some other alkaloids on the other. The latter always form triiodides. when iodine is added to an excess of a solution of their salt.1 1 Froc. Am. Phar. Assoc., 1898, Vol. 46, p. 35S. Abstract, this JOURNAL, Vol. 70, p. 439. |