340 ABSTRACTS OF CHEMICAL PAPERS ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOOD AND DRUGS ANALYSIS. Physical and Chemical Characters for the Identification of Aspirin. D. E. Tsakalotos. (J. Phrm. et de China., 1916, 14, 174-177.)-Aspirin crystallises in small well-characterised prisms. When heated over a flame on a glass slide up to but not beyond the melting-point, resolidification takes place, not in the form of prismatic crystals, but as concentric rings about round centres, the successive rings outwards being of increasing thickness. When heated to a temperature distinctly above the melting-point and cooled very gradually, solidification takes place in the form of a transparent vitreous mass.Fusion takes place with decomposition and liberation of acetic acid ; consequently, no definite melting-point can be given for aspirin; observations range from 125" C ., or even lower, up to 135" C., depending on the rate of heating. On heating for 1 hour at 130" C., the loss of acetic acid corres- ponds to the conversion of 66 per cent. of the aspirin into salicylosalicylic acid. With an aqueous solution of pure aspirin, freshly prepared, ferric chloride gives no coloration; but if the aspirin be heated to incipient fusion and then dissolved, the addition of a few drops of ferric chloride gives an intense violet coloration.When aspirin is heated above its melting-point and then dissolved in alcohol, the addition of water produces a white precipitate of salicylosalicylic acid, and a few drops of ferric chloride added to this gives a whitish-violet coloration.Some specific re- actions, according to Self, are given with a vanadic acid reagent. The author pre- pares this reagent without the addition of formaldehyde, thus: A small quantity of ammonium vanadate is dissolved in concentrated sulphuric acid ; an orange colour is produced, and water is added until this colour is weakened but not discharged.With this reagent, pure aspirin in the solid state shows no change a t first, but in a short time the reagent becomes yellowish-green and finally an intense green. Aspirin previously heated to incipient fusion gives an intense green immediately. Aspirin previously heated above its melting-point gives a dark green colour, which immedi- ately changes to brown. J. F. B. Esti.mation of Gum in the Officinal Syrup of Gum.E. Luce. (Ann. FaZsiJic., 1916,9,227-231.)-The test of Roussin, depending on the formation of a jelly on the addition of ferric chloride, gives only approximate indications or, if carried out so as to afford quantitative results, is very tedious. Two methods depending on the use of alcohol are more convenient: that of Rocques and Sellier, in which precipitation is performed in presence of lead acetate, is the more exact, while that of Bellier, where calcium chloride is employed, is simpler and sufficiently accurate for practical purposes.According to the method of Rocques and Sellier, 20 grms. of the syrup of gum are heated with 50 C.C. of water in a measuring flask and diluted to 100 C.C. Twenty-five C.C.of the solution are treated with 50 C.C. of 95 per cent. alcohbl, with constant stirring, and 2 C.C. of a saturated alcoholic solution of neutral lead acetateFOOD AND DRUGS ANALYSIS 341 Ratio ' Iodine Num- ' ber. 1 @anus). are added drop by drop. The precipitate is allowed to settle for half an hour, the liquid is decanted off through a counterpoised filter; the precipitate is washed by decantation with 50 C.C.of 75 per cent. alcohol in two portions, and transferred to the filter, where it is washed with 20 C.C. of 75 per cent. alcohol, then dried in the oven at 100"-110" C. for six hours. It is weighed dry, incinerated in a porcelain crucible with the paper, and the ash moistened with 10 drops of nitric acid. The residue is weighed as lead oxide, and the weight deducted from that of the pre- cipitate.The final result is multiplied by the factor 1.1764 in order to convert dry ash-free gum into terms of natural gum-arabic. According to Bellier's method, the syrup is diluted in the manner described above, and 20 C.C. of the solution are treated gradually, with stirring, with 40 C.C. of 95 per cent. alcohol and 1 C.C. of a 10 per cent.aqueous solution of calcium chloride. The precipitate is left t o settle for twenty-four hours and the liquid decanted off; washing is performed by decanta- tion with 60 C.C. of 65 per cent. alcohol, three times; the precipitate is transferred to the filter, and washed again with 20 C.C. of 65 per cent. alcohol. It is dried in the oven on the counterpoised filter paper and weighed dry.The dry weight, without correcting for ash, is multiplied by 1.1363 for the equivalent of natural air-dry gum. The results are slightly low (about 98 per cent. of the actual). Obviously these methods are only correct with pure gum syrups, free from dextrin. J. I?. B. Unsap- I Cloud- onified ing Matter. Point. 0 C. per Cell t . Philippine Beeswax. H. C. Brill and F. Agcaoili. (Philippine J .of Science, 1916, 11, 15-18.)-Thirteen samples of genuine Philippine beeswax (which is pro- duced by Apis xonata, A . dorsata, and d. indica) gave the following anaiyticai results after being freed from impurities by boiling with water, and dried at 100" C. : -__ _.___ Maximum .. Minimum .. Average . . sp. gr. 1 1 Saponi- at ,,2ft. fication 15.5" C. ,,C I Value.Acid Value, -__ 7.9 6.0 6.8 Ester Value, - _ 100.1 90.0 94.8 I - ' -7 ~ -I- 15.6 ' 10.8 i 58.6 60.0 12.4 I 7.4 51.6 59.0 13-9 9.0 1 55.7 59.6 I The clouding-point was determined by the method of Salamon and Seaber (ANALYST, 1915, W, 329). The melting-points are lower, and the saponification, acid and ester values higher than the corresponding values of Japanese and Korean beeswax (ibid., 1915, 40, 343).The percentage of unsaponifiable matter is some- what higher than the average value (52-38) given by Allen and Thomson for beeswax. C. A. M. Peroxidase Reaction in Milk. W. Grimmer. (Milchw. Zentr., 1915,44,246- 247; through J . Chern. SOC., 1916,110, ii., 403-404.)-The use of guaiacol and ethyl hydrogen peroxide is recommended for the detection of peroxidase in milk, since dilute solutions of these two substances remain stable for several years; they possess,342 ABSTRACTS OF CHEMICAL PAPERS therefore, a distinct advantage over guaiacum tincture and hydrogen peroxide solution.The test is carried out by mixing a few C.C. of milk with 2 drops of guaiacol solution (1 grm. of guaiacol dissolved in 10 C.C. of alcohol and diluted with water to 100 c.c.) and adding 2 drops of a 0.1 per cent.ethyl hydrogen peroxide solution. Unheated milk yields a brick-red coloration, whilst boiled milk remains colourless. The ethyl hydrogen peroxide may be prepared by the method described by Baeyer and Villiger ( J . Chem. Xoc., 1916, 110, I., 308). Quantitative Estimation of Morphine in the Various Organs when In- jected into Cats and Rabbits.A. W. Homberger and J. C. Munch. ( J . Amer. Chem. Xoc., 1916, 38, 1873-1876.)-Experiments are described which show that over 97 per cent. of the morphine administered hypodermically can be recovered by submitting the kidneys, liver, spleen, stomach, bladder and urine to analysis in the usual manner immediately after death. The proportion contained in the stomach is always small (1 to 3 per cent. of the total), but some is always found there.After 2 months’ burial, only 20 to 25 per cent. can be recovered, but from embalmed bodies as much as 70 per cent. can be recovered even after three months. For the analysis of the organs, Autenrieth’s modification (“ Detection of Poisons,” 1915, 57) of the Stas-Otto process was used with Puckner’s final ex- traction by hot amyl alcohol in slightly ammoniacal solution ( J .Amer. Chem. Xoc., 1901, 23,420). For the analysis of blood and urine, Dragendorff’s method (Blyth’s “ Poisons,” 1906, 313) was followed again with Puckner’s precautions (Zoc. cit.). G. C. J. Tin in Canned Foods. W. D. Bigelow. ( J . Ind. and Eng. Chem., 1916, 8, 813-815.) -The tin found in canned foods is usually assumed to be in solution, but the separate estimation of tin in the drained solids and in the liquor furnishes evidence that a large proportion of the total tin is present in an insoluble form, some also being present in the colloidol state (Chapman, ANALYST, 1913, 38, 472). The longer the food has been canned, the higher is the proportion of insoluble tin, tin originally in solution being slowly rendered insoluble. Results obtained in the study of the toxicity of soluble tin compounds cannot be used as a criterion of the toxicity of canned foods containing tin in an insoluble form, since in such a form it is probably far less readily absorbed from the intestinal tract (cf. Buchanan and Schryver, ANALYST, 1909, 34, 121). A number of analyses are quoted. H. F. E. H.