. Jour. Pharm

March,

substances (impurities) may be present in the solvents from which iodoform is recrystallized, thus contaminating the crystals, or they may be present in the solvents; such substances as retard the change, if present in minute quantity, are hydroquinone, pyrogallic acid, aniline, pyridine bases and aldehyde.-Pharm. Ztg., 1889, 31.

Fluorescence.-E. Geissler examined a yellow powder used for destroying the fluorescence of petroleum oils in the proportion of 0·2-0·3 gm. for 100 cc. oil; it proved to be nitro-naphthalin. Nitrobenzol also possesses this property although not to such a marked degree. The interesting observation was made that the fluorescence of quinine salts was destroyed by a little of these chemicals. If light be made to traverse solutions of these substances it will not produce the fluorescent effect either upon quinine solutions or petroleum oils; this is explainable by the possible absorption of the blue rays by nitro-benzol and nitro-naphthalin.-Pharm. Centralh., 1889, 11.

40 58 5

Russian turpentine from Pinus sylvestris contains about thirty per cent. of a crystalline acid C1HO, obtainable by extracting the turpentine with 50-60 per cent. alcohol and treating the granular residue with boiling alcohol, which solution solidifies to a crystalline mass on cooling. The acid is insoluble in water, soluble in alcohol, glacial acetic acid, ether and carbon disulphide; it melts at 143°, boils at 360°, and is converted by HCl into a modification melting at 159°160°.-W. Schkatelow, Apoth. Zig., 1889, 99.

Hyponitrous oxide or nitrogen monoxide can be obtained perfectly pure by heating 5 parts crystallized stannous chloride, 10 parts hydrochloric acid sp. gr. 1·21, 0·9 parts nitric acid sp. gr. 138, until the mixture boils, when a steady evolution takes place according to the reaction:

2HNO,+4SnCl,+8 HCl=4SnCl,+N,O+5 H,O.

3

The above proportions must be strictly adhered to.-G. Campani, Chem. Rpt., 1889, 5.

Cobalt and Nickel.-Krüss and Schmidt in redetermining the atomic weights of these metals by precipitating a neutral solution of auric chloride by means of metallic cobalt and nickel, obtained quite variable results, due to supposed admixture of Co and Ni with the precipitated gold. To control this error the gold precipitate was dissolved and reprecipitated by addition of sulphurous acid; even now the results were still discordant. In washing the gold precipitate the color of the washings disappeared and then became finally greenish;

this portion was collected separately and after evaporation and ignition a white oxide was obtained which, on examination, proved to be that of a new element. From 50 gm. oxide of nickel 1 gm. of this white oxide was obtained. The reactions of this new element are : white oxide soluble in HCl, which solution. on warming is green colored, on cooling again becomes colorless; hydrate insoluble in excess of the alkaline hydrates, but dissolved by fused KOH or Na OH; black sulphide in, alkaline solution, insoluble in ammonium sulphide; oxide non-reducible by H at high temperatures; chloride is colorless, but traces of HCl gas cause a green color which disappears when dissolved in water; chloride forms with red cobaltous chloride a double salt of green color.-Ber. d. d. Chem. Ges., 1889, 11.

Areca-nut contains three alkaloids, arecoline 0.07-0·1%, arecaine 0.1%, and the third one in such small quantity that it has not been possible to examine it. Arecoline, CH1NO2, identical with Bombelon's arecan, is an alkaline, colorless, oily liquid, soluble in water, alcohol, ether and chloroform; it is poisonous and probably gives the drug its tænifuge properties. Arecaine C,H,,NO2+H2O forms permanent colorless crystals soluble in water, insoluble in absolute alcohol, ether, chloroform, benzol, and appears to be inactive.-E. Jahns, Ber. d. d. Chem. Ges., 1888, 3404.

Amyl alcohol of commerce is always contaminated with furfurol and resinous matter, and is unfit for extraction purposes. To purify it, it is heated in a steam-bath with an equal volume of sulphuric acid for eight hours, the color changing to a black-brown; the alcohol is separated, neutralized with chalk and distilled in a current of steam. By repeating this process four or five times an almost pure amyl alcohol is obtained; perfectly pure (free from even traces of furfurol) it can only be obtained by decomposing potassium amyl-sulphate with sulphuric acid after first purifying the commercial salt by solution in alcohol and precipitation by a large excess of ether. Thus prepared amyl alcohol may be boiled for hours with concentrated sulphuric acid without assuming color.-L. Von Udranzky, Ztschr. f. physiol. Chem., xiii, 248.

Test for arsenic.-Flückiger in Arch. der Pharm., 1889, p. 1, critically examines Gutzeit's test and finds that it is decidedly more delicate than Marsh's test. The reaction is best carried out by generating hydrogen from dilute hydrochloric acid and zinc and allowing the gas after the addition of the arsenic solution to act upon filter paper moistened with

silver nitrate which is placed over the generator; the yellow coloration formed is due to Ag, As 3Ag NO,; this test will allow of the detection of 0.001 mg. As, O3. Not quite so delicate but a more convenient test is gotten by using mercuric chloride to moisten the filter paper, a yellow stain is also produced, but its nature is not established; 0.002 mg. As2O, will be indicated by this modification which has two important advantages: first, AgNO, is affected by light, HgCl, is not affected to any marked degree; second, H, Sb does not stain HgCl, while it does stain Ag NO. In alkaline solutions, by use of sodium amalgam, not less than 0.01 mg. As2O, can be detected; metallic aluminum with an alkali did not give good results as it contains either S, As or P, which interfere. Other metals in acid solution were tried but none were found superior to zinc. To test the zinc, 10gm. are acted upon by dilute HCl, the evolved gas should produce no yellow stain with Ag NO, or Hg Cl, in two hours, the test to be made in a dark place. The manufacturers of zinc are asked to produce a metal absolutely free from As, Sb, S and P.

Acetanilid in Phenacetin to the extent of two per cent. may be proven by boiling 0.5 gm. in 5-8 cc. water, allowing to cool, filtering, adding to the filtrate dilute nitric acid and a little potassium nitrite, boiling, adding several drops nitroso-nitric acid and again boiling; a distinct red color appears in presence of acetanilid.—Schroeder (Ned. Tydschr. Pharm.) Pharm. Ztg., 1889, 57.

1

Assay of narcotic extracts.—The method of L. van Itallie requires the following solutions: Lead acetate, 1:10; dilute sulphuric acid, 5:100; chloroform; ether; 6 normal acid; and as indicators cochineal tincture or an alcoholic solution of azotlinin or lacmoid. For the examination of aconite, belladonna and hyoscyamus extracts, the procedure is to take 5 gm. extract which is rubbed up with ten drops dilute sulphuric acid and sufficient water to make 50 cc., allowed to macerate one or two hours, and 25 cc. of the lead acetate solution added. After the subsidence of the precipitate, 50 cc. are filtered off through a dry filter, 10 cc. dilute sulphuric acid added, 50 cc. filtered into a separating funnel, sufficient ammonia added to give alkaline reaction and the alkaloid extracted by use of three portions of chloroform of 50 cc. each. The mixed chloroform extractions are distilled to dryness, the residue taken up in 5 cc. dilute alcohol and, after adding indicator, titrated with normal acid. The acid added represents the alkaloid in 23 gm. extract. For conium extract the

1

100

Jour. Pharm

,

solution is rendered alkaline by use of potassium hydrate (1:2) and for extraction of alkaloid ether is used in place of chloroform; before the distillation of the ether 2 cc. water should be added. 1 cc. 1 normal acid is the equivalent of 2.89 mg. atropine and hyoscyamine, 5.33 mg. aconitine and 1.27 mg. conine; to obtain the per cent. of alkaloid directly from the number of cc. acid used, the following factors are calculated atropine and hyoscyamine, 0·10404; aconitine, 0·1919; conine, 0.04572.

Control experiments with atropine recovered 98-62 and 99-71 per cent.-(Ned. Tydschr. Pharm.) Apoth. Ztg., 1889, 124.

Codeine used considerably in medicine of late is made synthetically by R. Dott by passing methyl chloride through a hydro-alcoholic solution of morphine and sodium hydrate; the alcohol is evaporated, the residue taken up in water and the codeine extracted with chloroform. A. Knoll (Pharm. Centralh., 1889, 39) introduces the methyl group into the formula of morphine by reacting upon the latter body with a salt of methyl-sulphuric acid. The product is dissolved in dilute sulphuric acid, the unchanged morphine precipitated from rather dilute solution by ammonia and from the filtrate the codeine is extracted by ether, benzol or chloroform. The alkaloid so gotten is pure and forms colorless rhombic prisms, melting at 155°, soluble in 17 parts hot and 85 parts cold water. For subcutaneous uses the phosphate is the best salt, being soluble in 4 parts water.

ABSTRACTS FROM THE FRENCH JOURNALS,

Translated for the AMERICAN JOURNAL OF PHARMACY.

PHENOLATE OF MERCURY.-On account of the variations observed in the preparation of this salt now in the market, M. Hugo Andres proposes the following method "by which pharmacists will always be able to obtain a definite product." First, prepare a phenolate' of potassium by dissolving in alcohol of 90 per cent., 94 parts of crystallized phenol and 56 parts of hydrated potash. Evaporate to a syrupy consistency in the water-bath, and place under a bell-glass with sulphuric acid until desiccation is effected. Then dissolve 100 parts of phenate of potassium in alcohol, filter, and precipitate the filtrate with an alcoholic solution of 112 parts of corrosive sublimate. The proportions are calculated as follows:

C12 H5 KO2 + Hg Cl = (C12 H3 O2) Hg + K CI.

. Jour. Pharm

March,

We thus obtain an orange precipitate, which should first be washed with alcohol of 60 per cent., and then with absolute alcohol until the filtrate gives no precipitate with sulphuretted hydrogen. The dried product is an amorphous powder of a brick red color with a faint odor of phenol. It is insoluble in water, chloroform, sulphide of carbon, ether and alcohol. With heat it dissolves easily in hydrochloric acid; with potash, the solution gives a precipitate of yellow oxide of mercury. It is also dissolved by nitric acid. The preparation contains 51-68 per cent. of mercury; theoretically it should have 51-81 per cent.J. de Ph. et de Ch.; Bull. com., January, 1889.

CAMPHORATED PHENOLS.-M. Désesquelle pointed out some time since (AMERICAN JOURNAL OF PHARMACY, 1888, p. 510) the liquefying influence of camphor upon naphthol. M. Audoucet has been testing the power of camphor over other phenols, and gives the results as follows: (The quantities of camphor cited represent the amounts strictly necessary to reduce the preparations to the condition of a soft paste); Resorcin, 2:50 gm.; camphor, 5 cgm.; Pyrogallol, 2:50 gm.; camphor, 10 cgm.; Thymol, 5 gm.; camphor, 1 gm.; Salol, 5 gm.; camphor, 50 cgm. An increased amount of camphor gives syrupy liquids miscible in all proportions with oils, lard and petrolatum, and which are soluble in alcohol and ether, and insoluble in water. Similar results were obtained with menthol.-Répert. de Phar., January 10, 1889.

PYRODINE. The proper doses of this antipyretic, said to be useful in pneumonia, sarlatina, typhoid fever, migraine and the neuralgias, are given by the Bull, méd. as follows: For children, the quantity to be given daily should be from 10 to 20 cgm.; for adults, 40 to 60 cgm. It should not be given oftener than every 18 or 24 hours. Administered repeatedly at short intervals it gives rise to toxic symptoms. It is said to be a powerful antiseptic as well as an antipyretic. Dr. Lepine proposes to call it phenacethydrazine, as, under its present name, it is likely to be coufounded with pyridine.-Répert. de Phar., January 10, 1889.

KAVAÏNE, ALKALOID OF KAVA-KAVA.-M. Lavialle (a pharmacist of Crest, France) writes to the Union Phar., Jan., 1889, that he has separated from kava an alkaloid which he has named kavaïne. He exhausted pulverized kava root with alcohol of 60 per cent., and distilled to the density of a fluid extract. He added distilled water to precipitate the resin, filtered the liquor, and neutralized it with ammo