THE ANALYST. 305 ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. Distinction between Raw and Heated Milk. Ute. (Oesterr. Chem. Zeit., 1904, vii., 389-391 .)-The author finds that the p-phenylenediamine tost gives a coloration with milk which has been heated at a temperature of 71' C. for one and a quarter hours. When the hydrogen peroxide is too concentrated the coloration is obtained even with boiled milk. The test, however, when properly performed, will detect 5 per cent. of mw milk in boiled milk. There is no advantage in using the reaction as a, zone test. Schardinger's test (methylene blue-formalin solution) is considered untrustworthy, w. P. s. The Composition of Dutch Butter. Grossmann and Meinhard. (Zeit. Untersuch. Nahr. Genussmittel, 1904, viii., 237-243.)-1n order to ascertain whether Dutch butters as a whole give abnormally low Reichert-Meissl values, the authors purchased in the open market (in Holland) fifteen samples of butter.The bulk of the butter was bought by large dealers for export to Germany. These fitteen samples were analysed, and gave Reichert-Meissl values from 29.5 to 33.4. The other analytical results also corresponded with those yielded by genuine bntters. It being the usual practice for dealers to " salt " the butter bought in the market before exporting it to Germany, samples were a few days afterwards taken in the latter country from consignments imported by the dealers mentioned above. These samples (fifteen) would correepond to the first fifteen samples. On analysis, how- ever, the Reichert-Meissl values obtained were considerably lower in every case- from 21.8 to 25.8.In some cases, the actual presencg of vegetable oil was proved by means of the phytosterol acetate test, and, from the results obtained in the other analytical determinations, all the samples might be considered as adulterated ones. From this it will be seen that Dutch butters do not always give low Reichert-Meissl values (Van Rijn, ANALYST, 1902, 136)' and that. exported Dutch butters are mixed with foreign fats at the same time that they are (' salted." w. P. s. Improvements in Gerber's Process for Fat Determination in Cheese. P. Wieske. (MilchrZeit., 1904, xxxiii., 353 ; through Chem. Zeit. Rep., 1904, xvii., 196.)-The improvement consists essentially in shaking the cheese (finely divided) with hot sulphuric acid.Four to five grammes of cheese are introduced into the butyrometer, and dilute sulphuric acid (specific gravity 1-500) added to about the 60 mark. The butyrometer is then placed in a water-bath at 70" to 80" C, and, on attaining that temperature, is taken out and well shaken. Repeated heating may be necessary for complete solution of the albuminoids. After cooling to 60" amyl alcohol is added, and the subsequent manipulation is as in the usual process. H. A. T.306 THE ANALYST. Detection of Rancid Fat in Edible Fats. F. Wiedmann. ( h i t . Untersuch. Nahr. Genussmittel, 1904, viii., 136-139.)-1t has been recognisd for some time that the rancidity of a fat or oil bears no relation to the amount of free fatty acid in the same.An oil with a high acid value may still be pleasant to the taste, or, in other words, be free from rancidity, whilst rancid oils may contain little free acid. Rancidity being due to the presence of products of decomposition possessing an aldehydic nature, the author proposes various tests for detecting these substances. On shaking 5 C.C. of melted fat with 5 C.C. of a 1 per cent. solution of phloroglucinol in acetone and 2 to 3 drops of concentrated sulphuric acid, the mixture is coloured red should even 1 per cent. of a rancid fat be present. It is thus possible to detect admixture of old and rancid lard with fresh lard. The coloration produced increases in intensity with the rancidity of the sample. Other substances, such as pyrogallol, p-phenylenediamine, guaiacum resin in the presence of acetic anhydride, etc., also give characteristic colorations with rancid fats.All the tests fail, however, with fats and oils which have been heated above 200° C. (see ANALYST, 1902, 363). w. P. s. The Dextrins occurring in Pine Honey. A. Hilger. (Zeit. Untersuch. Nahr. Genussmittel, 1904, viii, 110-126.)-These dextrins are readily precipitated from the honey by means of a mixture of methyl and ethyl alcohol, and have the character of achroodextrin. Each kind of pine honey contains a dextrin peculiar to itself, and having a constant specific rotation. The author has isolated the dextrins from four typical sorts of pine honey, and determined the rotatory power of each. The results obtained were : [aID = + 157.00 ; + 131.28 ; + 125.59 ; and + 119.90 respectively.The dextrin with [a],157 had the empirical formula C,HI,O,, exhibited true dextrin properties, and was scarcely attacked by dilute acids. Hydrochloric acid alone effected complete inversion. The remaining three dextrins were more closely allied to the sugars, and were readily hydrolysed by weak acids. Neither Fehling’s nor Ost’s solutions nor Soldiani’s reagent were reduced by the dextrins. After boiling for some time hydrolysis by the alkali took place, with a consequent reduction of the copper salts. The dextrin with [a],157 was not fermentable, and the others only with difficulty, little gas being evolved. Top and bottom fermenting beer yeasts, as well as certain wild species (Succharomyces and Sc hizosacchuromyces), acted more energetically on these dextrins than did the majority of the wine yeasts employed in the experiments. No osazone was obtained with any of the dextrins.w. P. s. Detection of Maize Flour in Bread. D. Ottolenghi. (Zed. Untersuch. Nuhr. Genussmittel, 1904, viii., 189-193.)-Although the detection of maize flour in wheat flour is a, comparatively simple matter, it is difficult to prove the presence of maize iu cooked materials, such as pastry, macaroni, bread, etc. For the latter purpose the following method is proposed, being based upon the separation of the proteids peculiar to maize, and recently investigated by Donard and Labbd : One hundred grammes of the bread (crumb) dried at a temperature of 4G0 C.THE ANALYST. 307 and finely powdered are treated for twelve hours with 500 C.C. of 0.3 per cent.potassium hydroxide solution, with frequent shaking. The liquid portion is then filtered through gauze, and the residue again extracted with the alkali solution. After three hours the whole is poured on the gauze, and the residue well pressed. The filtrate is evaporahed at a temperature not exceeding 70” C. When dry, the residue is broken up as finely as possible, transferred to a flask, and treated with 35 to 40 C.C. of absolute iso-amyl alcohol. The flask is attached to a, reflux condenser, and its contents boiled over an oil-bath for eix hours. After this time the amyl alcohol is passed through a filter while still hot, and the filtrate allowed to COO]. If the bread contains no maize, the yellowish-brown filtrate remains quite clear, or only slightly opalescent, buf in the presence of maize it becomes more or lese turbid.The addition to the filtrate of three times its volume of pure benzene causes no turbidity in the case of wheat bread, but accentuates the turbidity should maize flour be present. After allowing the filtrate to stand for twelve hours, the super- natant liquid may be decanted, and any precipitate redissolved in 2 C.C. of hot iso-amyl alcohol. On cooling, the solution becomes strongly opalescent, but not turbid if the bread consists of wheat flour, and very milky if maize be present. By adding 6 C.C. of benzene, iihe substance causing the milkiness is precipitated as yellowish flakes. w. P. s. Composition of Ducks’ Eggs. H. Liihrig. (Zed.Untersuch. Nahr. Genziss- mzttel, 1904, viii., 181-1$8.)-With a view to detecting the presence of ducks’ eggs in pastry, and also to ascertain the differences in composition between ducks’ and hens’ eggs, the authcr has carried out a, number of analyses, the results of which are given in this paper. Attention was principally paid to the determination of the lecithin- phosphoric acid contained in these two kinds of eggs (see ANALYST, this volume, p. 117). One hundred grammes of the yolk of ducks’ eggs were found to contain : Total phosphoric acid . . . . .. ... 1. Soluble in boiling alcohol ... ... Consisting of : ( a ) Directly soluble in efher . . . ( b ) Soluble in alcohol after extrac- tion with ether ... ... 2. Insoluble in boiling alcohol . . . ... (a) As nuclein ...... ... (b) As insoluble phosphates or compounds of phosphogly- ceric acid ... ... ... 1.255 grammes. 0.861 gramme (tot a1 dist earyllecit hin). 0.643 ,, (free dist earyllecithin). (disteary llecit hin com- 0.218 ,, { bined with vitellin). 0.394 ,, 0.178 ,, 0.216 ,, The chief differences between the above results and those yielded by hens’ eggs lie in the figures for free lecithin and that combined with vitellin. The average amount of ether extract obtained from ducks’ eggs (ten) was found to be: Total egg, 12.2 per cent. ; total egg, without shell, 13.7 per cent. ; and the yolk, 33.8 per cent. w. P. s.808 THE ANALYST. Determination of Xanthine Bases in Meat, Yeast, and other Extracts. 11. In Yeast Extracts (continued). K. Micko. (.&it: Untersuch. Nahr.Genuss mittel, 1904, viii., 227-237.)-Methods are given for the further purification of the fractions obtained by the process previously described (ANALYST, this volume, p. 158), the treatment employed following the lines of that given for isolating the bases contained in meat extracts (ANALYST, 1903, 315). The author has again investigated the alleged occurrence of carnine in meat extracts. In no instance was this base detected, the conclusion being that meat extracts do not contain it, or that it is of a transitory nature. Hypoxanthine was found to crystallize in two forms, one apparently as quadratic octahedra containing no water of crystallization. The other crystallizes as needles, which contain water, are unstable, and spontaneously change into the anhydrous form.w. P. s. Composition of Commercial Substitutes for Coffee. F. Duchacek. (Ann. de Chim. a?utZ., 1904, ix., 292-303.)-The following results were obtained in the analysis of three coffee substitutes manufactured in Austria, and of a sampIe of freshly roasted Ceylon coffee : Moisture ... ... ... Substances soluble in water Nitrogen soh ble in water ... Total nitrogen ... ... Sugars ... ... Dextrins ... ... Caffeine ... ... Ash ... ... ... Fat ... ... ... Cellulose ... ... Pentosans , . . ... Potassium oxide ... Sodium oxide ... Calcium oxide ... Phosphoric acid (P20s) Sulphuric acid (SO,) Silica (SiO,) ... ... Chlorine ... ... Lignin ... ... ... ... ... ... ~ .. ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ...... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... ... Ceylon Coffee. Per Cent, 1.96 26.02 1.74 1-10 1.43 0.90 1-12 3.65 15-05 20.92 7.18 16.27 2.22 0.06 0.22 0.49 0.15 0.01 0.04 Ma1 t Coffee. Per Cent. 2.07 41-93 1.86 0-36 1.73 15-82 3.19 5.24 7-50 2.108 8.35 0.38 0.06 0.12 1.09 0.07 0.84 0.03 - Fig Coffee. Per Cent. 7.83 70.99 1.19 0.71 35.70 2-30 4.47 3.07 0.91 5-17 2.13 0-44 0-53 0.68 0.17 0.08 0.05 - 5.a7 Chicory Coffee. Per Cent- 5.99 69.67 1.08 1.08 18.23 1-40 5988 2.23 8.13 4-21 9.21 3-08 0.41 0.25 0.48 0.05 0.89 0.16 - C. A. M. The Occurrence of Coffearine in Coffee. L. Graf. (Zeit. fur ofentl. Chem., 1904, x., 279-281.)-Paladino was the first to recogniae this new alkaloid (Berzchte, 1894, 406), and Forster and Riechelmann (ANALYST, 1897, 189) have also separatedTHE ANALYST.309 substance which they believe to be identical with coffearine. Doubt having been thrown by other observers on its actual occurrence in coffee berries, the author has repeated Paladino’s experiments, and obtained a substance having undoubted alkaloidal properties. It had the formula C,,H,,N20, and its hydrochloride crystallized from dilute alcohol in the form of needles, which contained one molecule of water of crystallization. The alkaloid was obtained from raw coffee beans, even when treat- ment with calcium hydroxide was dispensed with, showing that coffearine is not a, product of the reaction of the alkali on caffeine. It is present in the beans in very small amounts, and is not extracted from the decoction by chloroform, as is caffeine.w. P. s. The Composition of Chocolate Varnish. F. Jean. (Ann. de Chim. anal., 1904, ix., 258.)-A liquid preparation used in Spain for hardening chocolate and preventing it becoming white on keeping was found to consist of 25.6 grammes of gum benzoin, and 6.4 grammes of an unidentified resin in 100 C.C. of alcohol. C. A. M. A Fictitious Pepper. E. Collin. (Rdpertoire [3], xvi, 289; through Pham. Journ., 1904, lxxiii., 379.)-An ingenious fraud, consisting in the treatment of the seeds of a species of Pisum or Lathyrus to resemble black pepper-corns, is exposed by the author. The peas are apparently soaked in an aqueous extract of capsicums, and then treated with a dilute solution of an iron salt to give them a black colour.When mixed with pepper-corns the fictitious seeds are not readily detected by a cursory examination. The treated peas are also sold in the ground condition, powdered capsicum and olive stones being also frequently added. w. P. s. The Testing of Quinine Sulphate. B. H. Paul. (Chemist and Druggist, 1904, lxv., 428-430.)-The author takes exception to the British Pharmacopaeia test for cinchonidine in quinine, and suggests a method of procedure carefully worked out on the solubility limits, and depending on the appearance or non-appearance of crystals in the ether under precise conditions. The influence of quinine on the solubility of cinchoni- dine is also dealt with. The details of the method are as follows : 1 gramme of the quinine sulphate is dissolved in 100 C.C.of boiling water. After cooling the solution is filtered from the crystals of quinine sulphate and the filtrate evaporated to a bulk of 30 C.C. ; any further crystals separating are removed by filtration through a small plug of cotton-wool, and the filtrate made up to exactly 30 C.C. with water ; 5 C.C. of this solution are then treated with 5 drops of ammonia, and shaken in a corked tube with 1 c.c of ether. If at the end of one hour no crystals be formed in the solution, the quantity of cinchonidine in the 5 C.C. of solution would be less than 0.004 gramme, and consequently in original quinine sulphate less than 3.24 per cent. I n the more probable case of crystals being formed, less quantities (4.5, 4.0, 3.5 c.c.) are shaken out with ether and ammonia, until a difference amounting to 0.5 C.C.of solution corresponds to an entire absence of crystals in the one instance and a slight formation of crystals in the other after twelve hours’ standing. The mean of these310 THE ANALYST. two quantities is then. taken as containing 0.004 gramme of cinchonidine, and the percentage calculated on that basis. When shaken out from aqueous solutions, the ethereal solution becomes supersaturated, but deposits crystals on standing. A 'solution of quinine in ether is a better solvent for cinchonidine than ether itself, and coneequently the above method is so devised that the quantity of the quinine preeent is considerably reduced before applying the test. Cinchonidine has an abnormal solubility in ether. W. P. S.~ ~~ A Morphine Reaction, C. Reichard. (Phrm. Zeit., 1904, xLix., 523 ; through Chm. Zeit. Rep., 1904, xvii., 195.)-A small quantity of morphine, or one of its salts added to a mixture of formaldoxime sulphate with concentrated sulphuric acid, gives, on heating, an intense blue colour, even with quite minute traces of the substance. Atropine gives a brownish-black colour, disappearing on addition of water. H. A. T. The Identification of Colouring Matters in Absinthes. P. Onfioy. (Journ. Phamn. Chim., 1904, xx., 99-104.) The three principal colouring matters in genuine absinthe are chlorophyll, a vegetable yellow, and glycyrrhizin. In testing whether a sample contains only these colouring matters derived from the plants used in the manufacture, 200 C.C. of the liquid are evaporated until the alcohol is expelled.The residue should be turbid, and of a greenish-yellow colour. A clear aqueous residue indicates the absence of chlorophyll. The cold neutral liquid is twice shaken with amyl alcohol, which extracts the chlorophyll. The residual aqueous layer (which should be yellow) may contain glycyrrhizin. I t is concentrated to about 15 c.c., and treated with a few drops of sulphuric acid. This precipitates the glycyrrhizin in brown flakes, which are soluble in ammonium hydroxide, yielding a yellow solution. Many of the commercial samples of absinthe are weak in alcohol (35 to 40 per cent.), and hence cannot be coloured with chlorophyll, which is only stable in strong solutions of alcohol. I t is therefore replaced by artificial coal-tar colours, of which the most commonly employed are: soluble indigo carmine, solid yellow S, and a ponceau.The following dye-stuffs are also met with, though less frequently: Victoria blue, indulin blue, naphthol yellow, and Orange 11. In testing an absinthe containing a mixture of vegetable and coal-tar colours, 200 C.C. of the liquid are evaporated to dryness, the residue taken up with water, and the liquid filtered from the insoluble chlorophyll. If the filtrate has a blue or green shade, the presence of an artificial colour may be regarded as certain. This liquid is then extracted with amyl alcohol, giving an extract, A, and a residue, B. The extract A, which ought to be yellow (if blue, Victoria, blue), is evaporated to dryness, the residue taken up with water, and the liquid treated with a few drops of sulphuric acid, and again extracted with amyl-alcohol.The alcoholic extract is evaporated with a little unmordanted wool, the liquid being neutralized as exactly as possible with a few drops of ammonium hydroxide before complete evaporation. The residue, B, is evaporated in like manner with a little unmordanted silk. All colours that distinctly dye unmordanted wool may be regarded as coal-tar products. The following table gives the characteristic reactions of the different colours met with in commercial absinthe8 :Colouring Matters. Chlorophyll . . . Vegetable yellow Indigo carmine.. . Indulin blue ... Victoria blue ... Solid yellow S . . . Naphthol yellow Ponceau 3 R ... Orange 11. ... Glycyrrhizin .. . Solubility. Water. nsoluble soluble soluble soluble very soluble soh b 10 soluble soluble soluble soluble Ethyl Alcohol. very soluble soluble soluble soluble very soluble soluble soluble soluble soluble soluble Amy1 Alcohol Extract. Neutral. -______ rapid extraction, green slow extraction not extracted not extracted rapid extraction, blue extracted with difficulty extracted extracted with difficulty extracted not extracted -- Acid. yellow extract rapid ex traction greenish extract extracted rapid extraction blue extracted extracted extracted extracted not ex tract ed ~ _ _ _ Alkaline. -- yello w extract very slow extract ion not extracted not extracted rapid extraction red very slow extraction very slow extraction not extracted extracted not extracted Colour Reactions, Sulphuric Acid.._ - - brownish black violet blue reddish brown yellowish brown yellowish brown cerise red - Addition of Water. - - blue violet green, ;hen bluc orange dirty yellow reddish yellow yello wid brown - Hydro- chloric Acid. - yellow no change blue greenish yellow & brown orange makes colour paler no change irownisl yellow I Immonia. I yellow yellow rownisl violet red yellow yellow no change dark brown - A. Does not dye wool except when mordanted (alum 10 per cent., tartrate 5 per cent.). B. Dyes unmordanted wool. Sodium Iydroxide. yellow yellow rownish violet red no change yellow no change dark brown Sxtract. - A B B B k E C. A. M312 THE ANALYST, The Chemical and Physiological Assay of Digitalis Tinctures. G. Barger and W. V. Shaw.(Pharm. Jozmz., 1904, lxxiii., 249-254.)-1n the course of an examination of various digitalis tinctures prepared according to the directions of the British Pharmacopaeia, the authors made a comparative study of the two methods, chemical and physiological. The chemical part was limited to a determination of the digitoxin by Keller’s method (Bey., 1897,125). I n the physiological determina- tion of the activity of the tinctures and of the digitoxin obtained from them, frogs were used, the species being Rana tevzporaria. Comparative experiments were limited to frogs of approximately the same weight. The tinctures employed had an average of 3.4 per cent. of total solids and 0.0485 per cent. of “crude” digitoxin (Keller), or 0.031 per cent. of “pure” digitoxin. By making up a tincture containing a known amount of digitoxin (Merck), it was found that Keller’s method yielded less than one-half the digitoxin actually present.The minimum lethal dose of pure digitoxin (Merck) for frogs of 23 to 26 grammes in weight was 0.3 milligramme. By determining the minimum lethal close of the various tinctures, the actual amount of digitoxin in them was ascertained. The authors consider that at present the physiological method is the only reliable one for this kind of tincture. Digitalin and digitaleln were found to be much less toxic than digitoxin. w. P. s. The Distribution of Fat and Strychnine in Nux Vomica Seeds. H. W. Gadd and S. C. Gadd. (Paper read before the Brit. Pharnz. Co72j, Shefield, 1904.)-As Some trouble occurs in making the official liquid extract of nux vomica, on account of the fat which the seeds contain, the authors carried out a series of experiments to ascertain what portion of the seeds contains the most fat. For this purpose the seeds were freed from hairs, and analyses made both of the seeds and the hairy portion. The following results were obtained : Hairs ... ... ... ... ... 7.0 ... ... 0.5 Remainder of seeds ... ... 2.0 ... ... 1.5 FAT. STRPCHNIKE. Per cent. Per cent. Whole seeds (calculated) ... ... 2.25 ... ... 1.4 As the weight of the hairs amounted to about 5 per cent. of the whole, no material loss of strychnine would be caused by their rejection in making the liquid extract, whilst at the same time a considerable portion of the fat would be removed. The skins of the seeds were found to contain little fat, and there is therefore no advantage in rejecting them. I n making extracts from the hairs and the inner portions of the seeds, it was ascertained that the fat is more readily removed by alcohol (70 per cent.) from the hairs than from the denser portions. IT. P. s.