154 THE ANALYST. Morning {Evening ABSTRACTS OF PAPERS PUBLISHED IN OTHER 3 0 U R N A LS. 2.1 ,) 2.5 2-3 ,, 2.8 FOODS AND DRUGS ANALYSIS. (Oesterrekh. Chem. Zed., 1904, vii., 101, 102.)-The milk is passed through a filter made of the finest bolting-cloth (silk), the filter being previously moistened with water. The dirt collected on the filter is washed with water, then with alcohol and ether, and either dried before brushing off the filter into a weighing-vessel or washed off with water into a platinum basin, evaporated, and weighed. Of 502 samples of milk examined, 37 were dirty, and yielded by the above method from 6.9 to 110.5 milligrammes of dirt per litre of milk. The results of experiments with dry powdered cow-dung are given, which Determination of Dirt in Milk. M.Ball& show that the method is trustworthy. w. P. s. Composition of Goat’s Milk. P. Buttenberg and F. Tetzner. ( h i t . f6r Untersuch. der Nahr. und Genussmittel, 1904, vii., 270-272.)-The following table shows the variations in the composition of milk yielded by goats of different ages. The analyses extended over seven consecutive days : Age of Goat. Two years ... Two and a half years Three years ... Three years ... Five years ... Time of Milking. Per Cent. 3.8 to 4.4 4-9 ,, 5.6 3.4 ,, 3.7 4.0 ,, 4-7 Morning {Evening 3.1 ,, 3.4 Morning {Evening Non-fatty Solids. Per Cent. 8.82 to 9.07 8.59 ,, 8.99 8-19 ) ) 8.53 8.14 ,, 8-59 8.01 ) ) 8.43 8.18 ,, 8.52 8.02 ,, 8.23 7.91 ,, 8.38 7.13 ,, 7.71 7.37 ), 7.59 w. P. s. A New Method for Determining Cocoanut Oil in Butter. E.Polenske. (Zeit. fiir Udersitch. der Nahr. wid Genussmittel, 1904, vii., 273-280.)-The method described is based upon the determination of the volatile insoluble fatty acids which distil over in the ordinary Reiohert-Meissl procese. In order that concordant resultsTHE ANALYST. 155 may be obtained, the distillation must be carried out under certain conditions and in an apparatus of the dimensions of that shown in the illustration. For saponifying the 5 grarnmes of fat, 20 grammes of glycerol and 2 ca. of 50 per cent. sodium hydroxide solution are used. An alcoholic solution of the latter is to be avoided. After dissolving the soap and adding the requisite quantity of sulphuric :--- acid as usuaJ, the distillation is proceeded with. The flame is regulated so that 110 C.C.i of distillate axe obtained in from nineteen i to twenty-one minutes. The temperature ' of the condenser water should lie between 1 : 18" and 20" C. When 110 C.C. of distillate have been collected, the receiver is replaced by a 25 C.C. cylinder. Without mixing its contents, the receiver is placed in a bath of water at a temperature of 10" C . for ten minutes, the surface of the water being just above the 110 C.C. mark. The insoluble fatty acids rise into the neck of the flask, , and in the cage of butter form solid white opaque granules, whilst with pure cocoanut oil clear, oily drops are obtained. Mixtures containing more than 10 per cent. of cocoa- nut oil also yield oily droplets. After mix- ing and filtering the contents of the flask, the Reichert-Meissl value is determined on i 7 XI 7 the filtrate.The condenser, cylinder, and receiver are washed with 18 C.C. of water, which are then poured over the filter. The insoluble fatty acids on the filter are now dissolved in alcohol, and the solution titrated with barium hydroxide soluiion, using phenolphthalein as indicator. The number of C.C. of i; barium hydroxide solution required is termed the " new butter-value " of the fat under examination. Thirty-one various samples of butter, having Reichert-Meissl values between 23.3 and 30.1, gave '' new butter-values " from 1.5 to 3.0. Four samples of cocoanut oil, with Reichert-Meissl values from 6.8 to 7-7, gave L c new butter-values " from 16.8 to 17.8. Numerous analyses of mixtures are also given, from the results of which it is Been that butters with Richert-Meissl values between 23 and 27 give '' new butter- values " from 1.6 to 1.9, or a rise of 1.0 in the former is attended by an increase of 0.1 in the latter.The " new butter-value " in the case of butters hrtving Reichert- Meissl values of 28, 29, and 30 increases more rapidly-2.2,2-5, and 3.0 respectively. The rise, of course, is still more marked if cocoanut oil be present. The method is approximately quantitative if the Reichert-Meissl value of the sample be also taken into account. w. P, s.156 THE ANALYST. Reichert- Meissl \'slue. (a). Detection of Cocoanut Oil in Butter and other Fate. A. Juckenack and R. Pasternack. (Zeat. fur Untersuch. der Nahr. und Gentusmittel, 1904, vii., 193- 214.)-Although the presence of cocoanut oil in butter is not readily shown by the usual constants obtained in the analysis of the fat, the authors point out that by taking the relation of certain of these constants to one another, and also determining the molecular weight of the soluble and insoluble fatty acids, the detection of cocoanut oil is rendered more certain.For instance, on subtracting the saponifica- tion value from 200, and further subtracting the result from the Reichert-Meissl value, a figure is obtained which in the case of pure butters varies from -3.39 to + 4.14. The mean molecular weight of the volatile soluble fatty acids of butter varies from 95.0 to 99.0, and of cocoanut oil from 130.0 to 145.0. The molecular weight of the insoluble fatty acids of butter lies between 259.5 and 261.0, whilst the insoluble fatty acids of cocoanut oil have a mean molecular weight of 208.5 to 210.5.The phytosterol-acetate test is also of great value for detecting cocoanut oil, or other vegetable oil, in butter. In the following table ;L summary is given of the results of the analysis of a few typical samples : Pure cocoanut oil gives a figure from - 46.98 to - 50.71. St~ponifica- tion Value. '' Difference " n - ( b - 300). (a). Pure butter.. . ... Butter containing 10 per cent. cocoanut oil . . . ... ... Butter containing 20 per cent. cocoanut oil.. . ... ... Three commercial butters containing cocoltnut oil ... 27.51 25-27 24.06 24.40 19.20 24.35 ---_____- ~- 223.37 + 4.14 226.96 - 1.69 230.22 - 6.16 232.24 - 7.84 230.50 - 11.30 235.83 - 11.48 Pliytosterol- wetate Test. - - - - - 121.2O C." 115*oo c.t Molecular U'eight of the Non-volatile Fatty Acids. 260.15 ~ _ _ _ _ 254.06 249.02 248.79 246.41 247.99 w. P. s. An Organic Phosphorus Compound in Natural Wine and Qrape Stones. J. Weirich and G. Ortlieb. (Chem. Zed., 1904, xxviii., 153, 154.)-A wine pre- pared from grapes grown in the island of Thyra was found to contain 0.095 per cent. of phosphoric anhydride. Other wines examined contained from 0-02 to 0.06 per cent. As the proportion of nitrogen in a wine varies almost directly with the phosphorus, it is probable that the latter is present in the wine in the form of lecithin or similar compound which has its origin in the grape- stones. Strong natural Southern wines contain more organically combined phosphorus than do artificially prepared wines.Pure wines are sometimes pasteurized to improve their * After fifth crystallization. t After seventh crystallization.THE ANALYST. 157 keeping properties, but this is not to be recommended, as lecithin is decomposed at a temperature a little above 50' C. w. P. s. A Simple Method for the Defection of Citric Acid in Wine. A. Devarda. (Zeds. landw. 'Versuchsw. in Osterr., 1904, vii., 1 ; through Chem. Zed. Rep., xxviii., 42.)-By means of the following method 0.2 to 0.25 per cent. of citric acid can be recognised with certainty in wine: The alcohol is first boiled off, and the wine diluted to its original volume; 50 C.C. are then shaken for one minute with 2 to 4 C.C. of a 10 per cent. solution of pure malic acid and 1 to 2 grammes yellow mercuric oxide, and immediately filtered.To 40 C.C. of the filtrate 6 C.C. of 95 per cent. alcohol and 2 C.C. of mercuric nitrate solution are added, the liquid is shaken up a little and then allowed to stand for a few minutes in cold water at 10" to 15" C. The mercuric nitrate solution used is prepared by adding 2 C.C. of glacial acetic acid to 16 grammes of che salt, and gradually making up to 100 C.C. with water. The precipitate produced by the mercuric nitrate is filtered off, and, after the liquid has drained away completely, it is treated on the filter with 15 C.C. of 7 per cent. acetic acid, without shaking. Of the total filtrate, 10 C.C. are then treated with 1.5 C.C. of lead acetate solution, prepared by mixing 4 parts of a cold saturated solution of lead acetate with 1 part of glacial acetic acid.After heating the whole to boiling, it is filtered rapidly through a small washed filter-paper, and the filtrate allowed to cool slowly to 10" or 12' C. If the wine contains no citric acid, the filtrate will remain clear on cooling ; at the most a slight precipitate of lead tartrate is obtained after some time, insoluble on warming. If citric acid is present, on the other hand, the liquid becomes milky and opaque, and the precipitate only settles after a long time. A. G. L. Detection of Tartaric Acid in Citric Acid. 0. V. Spindler. (Chem. Zed., xxviii., 148.)-The words ( ( 2 C.C. dichromate solution 5 : 1,000 " in the author's paper on the " Detection of Tartaric Acid in Citric Acid " (Chem.Zed., xxviii., 15 ; ANALYST, this vol., 118) should read '' 2 C.C. dichromate solution 5 : 100." A. G. L. Breakfast Foods. J. B. Weems and C. E. Ellis. (Iowa State Coil. Agric. BdZetin, lxxiv., l01-114.)-Analyses are given of thirty-four kinds of these cereal preparations. The results show that the statements printed on the packages as to the value of the foods are greatly exaggerated. The preparations do not possess any nutritive value in excess of ordinary food materials. The claims made for many of the " predigested " foods are valueless, and no reliance can be placed in the state- ments that they are remedies for any disease, these foods not being medicines. w. P. s. The Determination of Gliadin in Wheat Flour by means of the Polmimeter Harry Snyder. (Journ.A w r . Chent. Soc., xxvi., 263.)-For the polarimetric158 THE ANALYST. determination of gliadin, 15-97 grammes of the flour are extracted with 100 C.C. of 70 per cent. alcohol, the whole being shaken every half-hour for two or three hours and then allowed to stand for twelve to eighteen hours at a temperature of 20" C. The time of extraction may be shortened by using a shaking machine and clarifying the liquid by centrifugal action, but excessive shaking is to be avoided as tending to give cloudy filtrates. The extract is filtered and polarized, using a 220 millimetre tube. On multiplying the reading on the sugar scale by 0.2, values for the gliadin nitrogen are obtained which agree very well with those given by a Kjeldahl determination on the alcoholic extract.It appears that flour of good quality should contain 12 per uent. of total proteids (N x 6.25) or about 11 per cent. of protein (N x 5*7), and that from 55 to 65 per cent. of the protein should be in the form of gliadin. A. G. L. Determination of Xanthine Bases in Meat, Yeast, and other Extracts 11. In Yeast Extracte. (Zeit. fiir Untersuch. der Nahr. uiul Genuss- mittel, 1904, vii., 257-269.1-The process used wad similar to that previously described for the determination of xanthine bases in meat extracts (ANALYST, 1903, 315). The acid employed for the preliminary boiling was more dilute than in the case of meat extract, 300 grttmmes of yeast extract being boiled with 2,300 C.C. of water and 200 C.C. of dilute sulphuric acid (1 : 3). The hydrochloric acid solution of the bases obtained from the copper bisulphite precipitate, after removal of the copper, was evaporated, and treated with ammonia.At the end of twenty-four hours the precipitate (Fraction I.) was filtered off. The filtrate was then precipitated with ammoniacal silver solution, as already described, and a dry residue of the bases obtained. Twenty-three grammes of the latter were dissolved in 1,250 C.C. of hot water, and mixed with 2,000 C.C. of hot picric acid solution (11 : 100). After cooling to 25" C. the precipitate was collected on a filter (Fraction 11.). .By evaporating the filtrate to about 300 c.c., and allowing it to stand for twenty-four hours, a furthei quantity of precipitate was obtained (Fraction 111.). The filtrate from this yielded still another amount of bases (Fraction IV.).These various fractions were purified and examined. Adenine, xanthine, and traces of hypoxanthine were also present. Adenine was the only bast detected in Fraction 11. I n comparison with the other fractions, Fraction 111. contained the largest quantity of xanthine ; hypoxanthine, guanine, and a small amount of adenine also being present. Fraction IV. consisted chiefly of hypo- w. P. s. I(. Micko. Fraction I. was found to consist principally of guanine. xanthine, with traces of xanthine, adenine, and guanine. The Amount of Sand in Cayenne Pepper (Paprika). R. Windisch. (Zeit. laidw. Vewuchsw. in Oesterr., 1904, vii., 19 ; through Chem. Zeit. Bep., 1904, xxviii., 55, 56.)-Sorne samples of cayenne pepper contain abnormal quantities of sand, although when examined under the microscope they appear to be genuine.Genuine oayenne should not contain more than 1.5 per cent. of sand at the outside, 0.5 perTHE ANALYST. 159 cent. being the average quantity. sample is adulterated. When the amount exceeds 1.5 per cent. the The total ash, less sand, of cayenne varies between 5-62 and 8.01 per cent., with an average of 7.01 per cent. w. P. s. Determination of Colchicine. (3. Bredemann. (Apot. Zeit., xviii., 817 ; through Pharm. Jown., 1904, Ixxii., 246.)-The following method, which is a modi- fication of Katz and Kremel's, is described for the determination of the active alkaloid in colchicum seeds. The coarsely-crushed seeds are extracted by percolating with 60 per cent.alcohol until about 10 times their weight of tincture is produced. Fifty grammes of the latter are evaporated to about 20 grammes, 0.5 gramme of paraffin wax and 20 grammes of water are added, the mixture is warmed until the paraffin melts, and the heating continued to evaporate the alcohol and reduce the liquid to about 10 grammes. After cooling, the whole is filtered, and the cake of wax washed with 10 C.C. of water and 1 gramme of acetic acid. The mixed filtrates are saturated with sodium chloride, and shaken out with chloroform as long as any alkaloid is removed. The chloroform extracts are filtered and evaporated to dryness. The residue is redissolved in water, filtered if necessary, evaporated, and dried over sulphuric acid. Seven samples of seed were found to contain from 0.45 to 1.34 per cent.of colchicine, and four samples of corm from 0.32 to 0.60 per cent. The coarsely- powdered seeds are somewhat, if only slightly, more easily exhausted than entire seeds, and percolation gives better results than extraction in a Soxhlet apparatus. w. P. s. New Reactions for the Detection of Cocaine. C. Reichard. (c'hem. .%it., 1904, xxviii., 299.)-The following tests are described: A trace of titanic acid is heated with tt few drops of concentrated sulphuric acid until dissolved, and cooled. On adding a minute quantity of cocaine hydrochloride to the mixture, no change takes place while cold, but, on warming, a violet or blue coloration is produced, according to the amount of cocaine salt added. When a trace of cocaine hydrochloride is mixed with a little solid potassium-ethyl sulphate and a drop or two of concentrated sulphuric acid, a powerful peppermint odour is produced on heating the mixture.A further test consists in warming a salt of cocaine with sulphuric acid and an organic amide, such as urea or ethylene-diamine hydrochloride, when a deep blue coloration is produced. w. P. s. The Correction for Increase of Volume in the Determination of Morphine in Opium and Tincture of Opium. E. Dowzard. (Pharm. Joum., 1904, lxxii., 397, 398.)-In a method recently published for the analysis of opium (ANALYST, this vol., p. 91) 51% C.C. of filtrate are used for the determination of the morphine, 1.6 C.C. being taken as the increase in volume due to extractives. This figure was calculated from the British Pharmacopaeia correction, but experiments have since proved that the increase in volume is much lower than that given in the British Pharmacopocia.160 THE ANALY8T.Eight grammes of opium were treated with 100 C.C. of water and 3 grammes of slaked lime, ae previously described. Five C.C. of the filtrate were rapidly evaporated and dried at 100" C. in a current of air free from carbon dioxide. After weighing, the residue was ignited, and the ash obtained assumed to be all calcium oxide, and calculated into Ca(OH), per 100 C.C. This was subtracted from the total extractive in 100 C.C. to give the amount of opium extract. The volume of the Ca(aH), and opium extract are calculated from the data : 3 grammes of Ca(OH), displace 1.44 C.C. of water, and 3 grammes of opium extract 1.9 C.C.of water. The sum of these two reeults gives the volume of the soluble matters in 100 C.C. of the filtrate, and this volume subtracted from 100 C.C. shows the amount of water present in 100 C.C. From this ia calculated the volume that the original 100 C.C. of water has increased to. In the case of tincture of opium, the increase given in the previously mentioned paper (2 c.c.) was correct. If the final volume be made up to 102 c.c., 50 C.C. of the filtrate The average result of a number of experiments was 0.9 c.c., not 1.6 C.C. correspond to 50 C.C. of the original tincture. w. P. s. Notes on AndrB's Reaction for Quinine. E. LBger. (Joz~rn. Pliarm. Chim., 1904, xix., 281-284.)-The emerald-green coloration produced on treating a solution of quinine with chlorine or bromine water followed by a&monia is widely employed as a qualitative test.The author, however, shows that under certain conditions the results may be very different. For instance, if 10 C.C. of a eolution of 0.5 gramme of quinine in 1,000 C.C. be shaken with 0.5 C.C. of a mixture in equal parts of saturated bromine water and distilled water, a yellow precipitate is formed and immediately redissolved, and on now adding 2 drops of ammonia solution and shaking the tube the normal emerald-green coloration is obtained. If, however, 1 c.,c. of the diluted bromine water be added in place of 0.5 c.c., a gooseberry-red colour is obtained, which, on standing, gradually disappears and changes to bright green. Or if to the normal green liquid in the first tube an additional 0-5 C.C.of the bromine solution be added the colour at once changes to violet. Conversely, if a trace of sodium bisul- phite be added to the red liquid in the second tube the colour immediately becomes green. Again, if 2 C.C. of the bromine solution be used in the test a yellow precipi- tate is produced, which gives a yellow opalescence on shaking. The addition of ammonia renders the liquid clear, but does not change the colour either to red or green. Hence the author concludee that it is necessary to keep the amount of bromine constant in this reaction, whereas the proportion of ammonia may be varied within wide limits. By using 0-5 C.C. of a bromine solution consisting of 1 C.C. of saturated bromine water in 200 C.C.of distilled water, it is possible to detect 1 part of quinine in 20,000. By working under identical conditions the reaction may be used quantitatively, provided quinidine be absent. C . A. N. Reagent for Myrrh. Hirschsohn. (Pharm. Ztg., xlviii., 96 ; through Pharnt. Joiim., 1904, lxxii., 247.)-Genuine myrrh, when treated with trichloracetal-chloral hydrate, gives a fine violet coloration. This reagent is prepared by passing chlorineTHE ANALYST. 161 into 75 per cent. alcohol, if possible in direct sunlight, until the liquid becomes cloudy and separates on standing into two layers. The lower of these is separated, washed with water, treated with magnesia to remove free acid, filtered, and mixed with four times its weight of chloral hydrate. The product is a syrupy liquid which fumes slightly. As far as the author's experience goes, no other resin or gum-resin gives the same coloration as does myrrh. w. P. s. Detection of Turmeric in Powdered Rhubarb, J. Anselmier, (Schueiz. Wochenschr. C l i e ? ~ . Phrm., 1904, xlii., 119 ; through Chem. Zeit. Rep., 1904, xxviii., 80.)-This form of adulteration may be detected by shaking 0.1 gramme of the powder with 20 drops of olive oil for one minute. One drop of the mixture is then placed on a white filter-paper, when a. characteristic yellow ring is formed should turmeric be present. The ring given by pure rhubarb cannot be mistaken for that yielded by turmeric. w. P. s. Determination of Resin in Gum Scammony. E. Dowzard. (Phar??z. J O I l T I L . , 1904, lxxii., 469.)-The following method is stated to be quicker than the usual one of extracting the scammony in a Soxhlet apparatus: Two grammes of the finely- powdered satnple are placed in a tightly-corked flask; exactly 20 c.c of ether are added, and the flask gently shaken until complete disintegration has taken plmx. After standing for fifteen minutes, with occasional ehaking, the ethereal solution is passed through a dry filter. Ten C.C. of the filtrate are then evaporated in a tared vessel, dried at 100' C., and weighed. Allowance is made for the fact that each 0.1 gramme of resin increases the volume of the ether by 0.075 C.C. w, P. s.