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Foods and drugs analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1906)
卷期: Volume 31, issue 361  

页码: 112-116

 

ISSN:0003-2654

 

年代: 1906

 

DOI:10.1039/AN9063100112

 

出版商: RSC

 

数据来源: RSC

 

摘要:

112 THE ANALYST. ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. A New Centrifugal Method for Determining Fat in Milk - Wendlep’s Method. Von Kuttner and Ulrich. (Zeit. ofentL Chem., 1906, xii., 41-58.)-The process consists in mixing the milk with a saline solution, adding a little isobutyl alcohol, and subjecting the mixture to centrifugal action, the procedure being similar to that of Gerber’s method. The saline solution employed contains tartrates, sodium chloride, and sodium hydroxide (proportions not given). Eleven C.C. of this solution, 10 C.C. of the milk to be tested, and 0.6 C.C. of isobutyl alcohol are successively intro- duced into a butyrometer tube and the latter then closed with an indiarubber stopper. The contents of the tube are mixed, the tube is immersed for two or three minutes in water at a temperature of 45” C., and then submitted to centrifugal action in the usual way.The surface separating the fat from the saline solution is quite horizontal, rendering the reading of the volume of the fat an easy matter. If the contents of the tube have been well mixed, no flocculent layer ever occurs between the fatty and aqueous layers. The results obtained, as shown by 360 comparative determinations, agree with those yielded by Gerber’s method. w. P. s. A Rapid Method for the Detection of Traces of Zinc in Wort, Beer, Wine, etc. J. Brand. (Ztschr. ges Brauw., 1905, xxviii., 440; through Chem. Zed. Rep., 1906, xxx., 25.)-The liquid to be examined is acidulated with hydrochloric acid, and a few drops of potassium ferrocyanide solution are added.The presence of even a, trace of zinc will cause a flocculent precipitate of zinc ferrocyanide to be produced, which, being mixed with much albumin, settles rapidly, and may be readily filtered after decanting the bulk of the liquid. The washed precipitate is ignited, and theTHE ANALYST. 113 residue treated with acetic acid; in the solution obtained zinc is identified with hydrogen sulphide. As little as 1 part of zinc in 500,000 parts of beer, etc., can be readily detected by this method. A. G. L. Hordenine: A New Alkaloid extracted from the Germ of Barley. E. Leger. (Journ. Pharm. Chim., 1906, xxiii., 177-181.)--A crystalline alkaloid has been separated by the author from the dried germs of malted barley.It was first obtained in ethereal solution by meam of Stas' method, and the residue left on evaporation purified by repeated crystallization from alcohol and decolorized with animal charcoal. The yield of hordenine appears to vary with the temperature at which the malt was dried, and the author has obtained from 0.22 to 0.45 or 0.5 per cent. from different germs. The alkaloid crystallizes in orthorhombic prisms, which show double refraction. They are anhydrous, colourless, and almost tasteless, and melt at 117.8' C. (corr.) to a colourless liquid. Hordenine slowly sublimes at its melting-point and rapidly at 140' to 150'. It is readily soluble in alcohol, chloroform, and ether, less soluble in benzene, only slightly soluble in water, and almost insoluble in cold petroleum hydrocarbons. It dissolves easily in hot carbon tetrachloride, but separates out almost quantitatively on cooling.It acts as a, strong base, giving a red coloration with phenolphthalein and displacing ammonium from its salts in the cold. It gives no coloration with strong sulphuric acid, and is hardly attacked by a hot concentrated solution of potassium hydroxide. On the other hand, it reduces potassium permanganate in acid solution, hot silver nitrate solution, and iodic acid solution, yielding a precipitate of iodine. Its formula, calculated from the composi- tion of its salts, is C,,H,,NO. I t is a tertiary monoacid base, and thus forms only a, single series of salts, all of which are very soluble in water. C. A. M. Determination of Chloral Hydrate.T. E. Wallis. (Pharm. Journ., 1906, vol. 76, 162, 163.)-The method proposed consists in heating the chloral hydrate with sodium hydroxide in alcoholic solution and titrating the sodium chloride formed. The determination of the amount of sodium hydroxide absorbed gives untrustworthy results (cf. ANALYST, 1903, xxviii., 189), unless strict conditions be adhered to. The details of the method are as follows : A weighed portion of from 0.1 to 0.4 gram of the chloral hydrate is dissolved in about 10 C.C. of the alcohol, and introduced into a, thick-walled bottle. A measured volume of $ sodium hydroxide solution is added, the bottle is closed by an indiarubber stopper, which is tied down, and the bottle with its contents heated for three hours in a water-bath. After cooling, the solution is neutralized with sulphuric acid, using phenolphthalein as indicator, and then titrated with & silver nitrate solution.The reaction is represented by the equation, CCl,CH(OH), + 5NaOH = 3NaC1+ 2HCOONa + 3H20. I t is important that the contents of the bottle during the heating contain at least 50 per cent. of alcohol by volume. w. P. s.114 THE ANALYST. The Determination of Traces of Chloroform. M. Nicloux. (Comptes Rendus, 1906, cxlii., 163-165.)-Chloroform when present in alcoholic solution in a quantity not exceeding 0.1 gram can be determined by diluting the liquid to 60 C.C. with alcohol, and boiling it for an hour under a reflux condenser with 10 C.C. of a 10 per cent. alcoholic solution of pure potassium hydroxide. When cold, the contents of the flask are mixed with 15 C.C.of water, exactly neutralized with phenolphthalein as indicator, and treated with potassium chromate, and the chlorine titrated with standard silver nitrate solution (8.535 grams per litre), each C.C. required representing 2 mgms. of chloroform. Air containing chloroform is analysed by being drawn through alcohol (95 per cent. strength), contained in two absorption vessels, at the rate of 1 litre in half an hour, and the absorbed chloroform is then determined as above described, In the case of blood and aqueous liquids it is necessary to add strong alcohol (80 to 95 per cent.), acidified with 0.25 gram of tartaric acid in the proportion of 5 parts to 1 of the sample, and to distil the mixture in a fractionating flask until about third has passed over.The distillate is received in 10 C.C. of 95 per cent, alcohol, and the chloroform determined as before. The results thus obtained are invariably 1-5 to 2 per cent. too low. C. A. M. The Constituents of Myrrh. A. Tschirch and W. Bergmann. (Archiv. Pharm., ccxliii., 641 ; through Pharm. Journ., 1906, vol. 76, 128.)-Picked Somali myrrh was found to have the following composition : Soluble in alcohol (resin and oil), 28 to 30 per cent, ; insoluble in alcohol (gum and enzyme), 61 per cent. ; im- purities, 3 to 4 per cent. ; moisture, 5 per cent. Part of the substances soluble in alcohol was insoluble in ether, the remainder (about 21 per cent. of the myrrh) being soluble. The portion insoluble in ether was redissolved in alcohol, and separated by precipitation with lead acetate into a-heerabo-myrrholol and P-heerabo-myrrholol, the latter remaining in solution. These substances were obtained in the form of yellowish-brown and grayish-brown amorphous powders respectively.The portion of the alcoholic extract soluble in ether was dissolved in this solvent, and treated with potassium hydroxide to remove a-and 6-heerabo-myrrhol, which were afterwards separated by means of lead acetate, when they were obtained as grayish-yellow powders, The ethereal solution was next evaporated and distilled in a current of steam. By this means a residue of heerabo-resene was obtained in the retort, whilst the distillate consisted of yellow oil. The latter had a specific gravity of 1.046, rapidly resinified, and bore no relation to the resin acids, resinotannols, resinols, etc., found in other resins.The substances insoluble in alcohol, consisting of the gum and enzyme, could not be separated from one another. In addition to these substances, myrrh also contains a bitter principle, but all attempts to isolate it failed. The gum yielded arabinose on hydrolysis. w. P. s. Determination of Cinnamic Acid in Storax. D. Hooper. (Pharm. Journ., 1906, vol. 76, 107.)-The determination of the amount of cinnamic acid in storax is proposed as a method of detecting the presence of adulterants in this balsam.THE ANALYST. 115 Tschirch and Itallie have shown that true Oriental storax contains 23 per cent. of cinnamic acid, and other investigators have concluded that the percentage of the acid should not fall below 20.A weighed quantity of the storax is saponified in alcoholic solution with potassium hydroxide, evaporated to remove the alcohol, the residue dissolved in water, and the solution shaken out with ether to remove unsaponifiable substances. The solution is then treated with sulphuric acid in excess, and the voluminous precipitate collected on a filter and washed. The precipitate is next dissolved in hot water, and the crystals which separate on cooling are collected, dried, and weighed. w. P. s. Adulterated Santal-Wood Oil. E. J. Parry. (Chemist alzd Druggist, 1906, lxviii., 211.)-The low price of large parcels of this oil imported from Germany caused suspicions to arise as to the purity of the oil, and the author has recently examined a sample which enabled him to definitely decide the nature of at least one of the adulterants present.The oil had a specific gravity of 0.970 a t 15' C., an optical rotation of - 14' in a 100 mm. tube, was soluble in 5 volumes of 70 per cent. alcohol, and had an apparent santalol value (free) of 93.5. By repeated fractionation under reduced pressure a small amount (about 5 per cent.) was obtained, which boiled at 220' C. at ordinary pressure. The specific gravity of this fraction was 0,943, and the refractive index 1.4823 a t 20' C. The odour left no doubt as to its being terpineol. This was confirmed by the melting-point (115' C.) of the nitroso- chloride yielded by the fraction. w. P, s. The Purity of Balsam of Peru, Utz. (Phar?n. Post,, xxxix., 21 ; through Pharm.Jouriz., vol. 76,129.)-Adulteration of this balsam is, according to the author, the rule rather than the exception. Turpentine and gurjun balsam appear to be the favourite adulterants, and the usual tests often fail to detect them. Such adulterated balsams may show a cinnamein content of 50 to 60 per cent. The physical characters of the cinnamein obtained sometimes indicate sophistication. It should be brown and homogeneous, whereas with turpentine it is often granular or even solid. The refractive index gives more satisfactory results, as for pure balsam the value varies from 1,5862 to 1,5878 at 15' C. ; whilst the refractive index of gurjun balsam is 1.5142; of castor oil, 1.4809; and of paraffin oil, 1.4821. On the other hand, perugen, which is a factitious substitute for balsam of Peru, possesses a refractive index of 1.5863. Perugen, however, gives an intense olive-green coloration with Ccesar and Loretx's nitric acid test, instead of the golden yellow yielded by pure balsam of Peru. TOXICOLOGICAL ANALYSIS. Toxicity of Cyanogen Compounds towards Fish. J. Hasenbaumer. (Zed. Uutersuch. Nahr. @eizussn%., 1906, vol. 11, 97-101.)-The author has carried out a considerable number of experiments regarding the action on fish of certain cyanogen compounds when the latter were added to the water in which the fish lived, The investigation was in connection with an inquiry regarding the discharge of effluent containing traces of these compounds. Potassium cyanide was found to be extremely w. P. s.116 THE ANALYST. poisonous to fish, 0.0018 gram per litre of water killing tench and goldfish in a very short time The following quantities per litre of other cyanogen compounds also killed fish of these species : Potassium ferrocyanide, from 1-5 to 3.0 grams ; potassium ferricyanide, from about 1.7 grain ; potassium or ammonium thiocyanate, about 1.5 gram. w. P. s.

 

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