water to about 75 c.c., filter through a tared Gooch crucible, dry to constant weight at 115° C., and weigh. The weight of the insoluble matter (tetrachlorfluorane) does not exceed 0.2 per cent. The ash, on incineration, should not exceed 0-15 per cent.

Phosphorized Oil, Determination of free Pin. O. Frey. (Pharm. Monatshefte, 1922, 3, 101, through Chem. Abstr., 1923, 17, 181.) Into a 200 Gm. medicine bottle weigh accurately about 15 Gm. of the sample, dissolve in a mixture of 10 Gm. of 96 per cent. EtOH and 30 Gm. Et2O, adding from a pipette 20 c.c. N/10 I, then cork the bottle and shake vigorously for 2 minutes. Run a control in another bottle with all the above ingredients except the oil. Titrate the I excess in both cases with N/10 Na2S2O3. Each c.c. of N/10 I used up = 0.001033 Gm. of free P. (See also Y.B., 1912, 160.)

Phosphorus Pills. Improved Formula for the Mass. E. А. М. Knott. (Pharm. J., 1923 [4], 56, 243.) The present official mass can be made without much difficulty, but most dispensers when making a dozen or two of the pills have trouble in piping, cutting and rounding, owing to the mass so readily softening and even melting in the hands. The following formula is suggested as being a more expeditious method, the mass is easier handled and has the further advantage that it can be kept immersed in water unchanged for months: Phosphorus, 1 gramme; calcium phosphate, 69 Gm.; wool fat, 30 Gm.; carbon disulphide, 20 Millilitres. Place the wool fat in a mortar, dissolve the P in the CS2, triturate the solution and the wool fat together, incorporate the calcium phosphate and work into a suitable mass. The mass may be kept immersed in water, or rolled, cut into pills, rounded and varnished. Where suitable, when ordered in combination with other ingredients, the equivalent weight of calcium phosphate might be omitted, thus securing a pill of small size without loss of active constituent. Objection may be taken to the use of calcium phosphate on the ground that soluble acid phosphate may be formed in the alimentary canal. It could, no doubt, be replaced by kaolin, but in practice it has been found that a mass made with kaolin is less satisfactory to handle and tends to crumble.

Quinine Ethyl Carbonate, Characters and Tests for. (New and Non-official Remedies : J. Amer. Med. Assoc., 1923, 86, 1617.) The tests recommended are practically the same as those of В.Р.С., 1911, except that the m.p. is given as 89-91° C. (В.Р.С., 95° C.).

Rhamnus Frangula Bark and its Preparations, Variation in the Amount of Oxymethylanthraquinones in. E. Maurin. (Bull. Sci. Pharm., 1922, 24, 175.) Although Rhamnus frangula is one of the most widely used aperients, its intensity is found to be uncertain. The investigations of the author indicate that this is due, as anticipated, to variations in the amount of free and combined oxymethylanthraquinones present. The age of the bark has an important bearing on the activity of the drug. It is at its maximum activity at the age of 3 to 4 years. Very young bark is less active; and, again, when 5 or 6 years old the amount of active principles again diminishes. The bark of young shoots 1 year old contained 0.3 per cent. of free, and 1.1 per cent. of combined oxymethylanthraquinones; that of branches, 3 years' old, 0.85 per cent. and 1.85 per cent.; that of 6 years old trunks, 1.25 per cent. and 0.60 per cent., respectively. Buckthorn bark from different geographical sources also showed considerable variation, from 3.2 per cent. of total anthraquinones in bark from Morvan to 2.70 in bark from Bavaria. The period of keeping the bark also has a very marked influence on the activity, since the combined anthraquinones show a considerable and increasing diminution with age. Thus, bark which was gathered in 1913 gave 1.75 per cent. of free, and 1.05 per cent. of combined anthraquinones; in 1919, 1.10 per cent. of free, and 1.8 per cent. of combined; in 1920, 0.8 per cent., and 2.15 per cent.; in 1921, 0.65 per cent., and 2.35 per cent. These figures indicate that the glucosides, which are the most valuable of the active principles, undergo considerable hydrolysis on prolonged storing. [This seems to indicate that the assumption that Rhamnus frangula bark improves by storing for at least a year is not well founded.-Ed. Y.B.]

The two chief galenical preparations of buckthorn bark are the fluid extract and the aqueous extract. Calculated on the equivalent of 100 Gm. of bark, the fluid extract was found to contain 2.8 per cent. of total anthraquinones, of which 0.85 per cent. were free. The aqueous extract equivalent to 100 Gm. of bark contained 2.1 of total and 1.25 per cent. of free anthraquinones. This shows that during the process considerable hydrolysis of the glucosides has occurred, and that the fluid extract is the better preparation. The tincture equivalent to 100 Gm. of bark gave a total anthraquinone content of 2.6 per cent., with 0.75 per cent. free. It is therefore a fair preparation, but a very large dose would be requisite to give adequate results. The decoction is richer than the infusion in anthraquinones ; those in the free state are practically the same in quantity in the two preparations. For determining the anthraquinones in these experiments the author has used the quantitative method described by him last year. (Y.B., 1922, 106.)

Santonin Tablets, Assay of. M. François. (J. Pharm. Chim., 1922, 26, 330.) Ten tablets are rubbed to very fine powder in a mortar, then triturated with 10 Gm. of CaO for 15 minutes. The intimate mixture thus obtained is transferred to a conical flask. Fifty c.c. of EtOH 95 per cent. is added, and the mixture is heated, under a reflux tube, on the water-bath just below its b.p. for 1 hour. The liquid is then decanted into another flask, through a filter, and the insoluble residue is twice extracted with more EtOH 95 per cent. in a similar To the bulked filtrate, 100 c.c. of water is added, and the EtOH is distilled off. The aqueous residue of this distillation is transferred to a separator, acidified with 10 drops of HCl, then shaken out with six successive 20 c.c. of CHCl3. These CHCl, extracts are bulked in another separator and shaken out once with 20 c.c. of water to remove any sugar that may be present. The CHCl, is then passed through a dry filter into a tared glass capsule and allowed to evaporate spontaneously in the dark. The residue is weighed as santonin. When about 1 Mgm. on a microslide is examined under a low power, it will be seen to be composed of characteristic striated rectangular crystals. On adding a few particles of pure KOH to this and gently warming the slide over a minute flame, when the KOH melts it will show bright carmine red streaks: and on again examining under the microscope the santonin crystals will be seen to be coloured red, without being dissolved. If a particle of the minute fused mixture is dropped into EtOH 95 per cent., it will give a red solution. Chocolate Santonin Tablets. The above method answers equally for these with the following slight modification. The process is conducted exactly as above until the EtOH is distilled off. It will then be found that the aqueous residue contains a little suspended fat. The liquid must therefore be thoroughly cooled, and carefully filtered while cold, before acidifying with HCl and shaking out with CHCl3.

Snow White Liniment. O. H. Hand. (Drugg. Circ., 1922, 66, 311.) Ammonium carbonate, 1 ounce; water, 8 ounces; white Castile soap, 6 drachms; hot water, 16 fluid ounces; camphor, 1 ounce; alcohol, 1 ounce; oil of turpentine, q.s. Dissolve the ammonium carbonate in 8 ounces of water, dissolve the Castile soap in the hot water and mix. Dissolve the camphor in the EtOH and add to the first made mixture, then shake. Add the turpentine in sufficient quantity (to form a cream emulsion), gradually adding it and shaking until an emulsion of creamy consistence results. (See also Y.B., 1907, 256; 1911, 332; 1914, 226; 1916, 376; 1921, 239, 283; 1922, 290; and Gen. Index.)

Sodium Chaulmoograte or Gynocardate, Preparation of. Н. С. Т. Gardner. (Pharm. J., 1922 [4], 55, 154.) After reviewing the chemical and pharmaceutical literature of chaulmoogra oil and its preparations, the following process for the preparation of the desired sodium salts is suggested as a result of practical experience. Commencing with, say, 80 lb. of Taraktogenos oil, about 14 lb. of commercial NaOH will be required for saponification. This amount should be dissolved in sufficient water to form a lye sp.g. 1.220. The oil is added to the lye and the mixture boiled for at least 6 hours with occasional stirring. When cooled, 7 lb. or so of NaCl is stirred in to salt out the soap. The soap is removed when cold and is dissolved in sufficient water. The fatty acids are liberated by the cautious addition of 31 lb. of H2SO4, sp.g. 1.530, stirring well for a quarter of an hour. If necessary apply heat. When cold, the fatty acids will form a compact mass on the top of the aqueous liquid. They should be removed and dissolved in 9 or 10 gallons of industrial EtOH; usually 91 gallons suffices. In order to eliminate as completely as possible the fatty acids of higher melting-points, the temperature of the EtOH solution is gradually reduced to 8° to 12° C. and maintained thereat for some hours. The fatty acids which have separated are removed, pressed, the expressed liquor returned to the bulk EtOH solution. It may be necessary to again reduce the temperature and proceed as before. The EtOH, liquor containing the remaining fatty acids, should now be transferred to a vacuum still and the EtOH distilled off under as greatly reduced a pressure as possible. When the fatty acids are completely dry their m.p. must be determined. This should be from 32° to 34° C.; if higher, the

FF

acids will have to be redissolved in EtOH and the whole process repeated until they exhibit a m.p. within this range. It has been found that the sodium salts prepared from the fatty acids melting between 32° and 34° C. are quite satisfactory for therapeutic use and are water-soluble. The EtOH recovered on distillation can be used for dissolving the fatty acids of the correct m.p. for the purpose of converting them into their Na salts. This is achieved by making a concentrated solution of NaOH-about 9 lb. will be required-in a small amount of water and neutralizing the alcoholic solution of the acids with it. Before, however, proceeding to do this a little of the solution of the fatty acids should be withdrawn and set aside to correct, if necessary, any slight over-addition of alkali. A little phenolphthalein solution must be dropped into the alcoholic fatty acids solution, then the NaOH solution slowly and carefully added, with constant stirring, until the acids are neutralized. Should too much NaOH be inadvertently added, some of the set-aside fatty acids solution should be added to neutralize this excess. The solution is now to be transferred into the vacuum still and the solvent distilled off at the lowest possible temperature. Care should be exercised that the temperature of distillation does not exceed 80° C., otherwise a dark brown product will be obtained. If the salt requires drying upon removal from the still, contact with Fe must be avoided, or the salt will materially deepen in colour even to a dark brown. Drying is best conducted by spreading on muslin trays placed in a room through which a current of warm dry air circulates. Finally, the Na salt must be powdered, sifted through a "60" sieve, and stored in airtight stoppered bottles.

Solutions Easily Oxidizable, Preservation of. M. Bridel. (J. Pharm. Chim., 1923, 27, 147.) It is found that by using as a solvent a 2: 1000 solution of benzoic acid in distilled water, and finally adding NaHSO3 solution sp.g. 1.30 in quantities not exceeding 3 c.c. per litre, the product will keep unaltered in colour, and in most cases may be sterilized at 110° C. for 20 minutes without showing any evident signs of decomposition. It is recommended for preparing solutions of novocain, emetine, apomorphine, physostigmine, and sodium salicylate. By this means it is possible to prepare ampoules of perfectly colourless solutions. (See also Y.B., 1922, 237.)

Sparteine, Quantitative Determination of, in Tablets. P. W.