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Foods and drugs analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1908)
卷期: Volume 33, issue 386  

页码: 188-191

 

ISSN:0003-2654

 

年代: 1908

 

DOI:10.1039/AN9083300188

 

出版商: RSC

 

数据来源: RSC

 

摘要:

188 THE ANALYST. ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. Estimation of Alcohol in Concentrated Nitrous Ether. W. A. Pearson. (dmcr. Jozwn. Pharm., 1908, 80, 101-105.)-Twenty to 35 grams of the preparation are rapidly weighed into a 200 C.C. flask containing ice-cold water, and the flask immediately connected with an upright spiral condenser, into the top of which is poured ice-cold water. If the lower opening be quite small, a spiral column of ice- water will be held in the condenser by the pressure developed by the volatilising nitrous ether. The ethyl nitrite evaporates at the ordinary temperature in about three days under these conditions. An alternative form of apparatus is one in which the vapours from the flask are made to pass through a series of five small wash- bottles contaihing ice-cold water.When volatilisation of the nitrite is complete, the solution in the condenser or wash-bottles is mixed with the liquid in the flask, and diluted to such volume that 20 C.C. contain about 0.1 to 0-3 gram of alcohol. The alcohol in 20 C.C. of solution is then determined by the method of DuprB, which consists in oxidising the alcohol to acetic acid by chromic acid and distilling the acetic acid from the liquid after destroying the excess of chromic acid with metallic zinc. The usual corrections for traces of sulphuric acid carried over in the distillation, and for any aldehyde or unvolatilised ethyl nitrite in the liquid before oxidation, should be made. A, R. T. Simple Method for the Estimation of Alcohol in Distillery Wash by Means of the Zeiss Immersion Refractometer.B. Wagner, F. Schultze, and J. Rub. (Chem. Zeit., 1908, 32, 297-298.)-The method consists in determining the refractive index on 5 or 10 C.C. of the filtered wash, and also determining the refractive index of 20 C.C. of the same solution after evaporating to 10 C.C. to expel the alcohol, and making up to 20 C.C. with distilled water. The difference of the two result8 is added to the value for the refractive index of water at the temperature used, the percentage of alcohol present being found by reference to II table contained in the original paper. For accurate work a correction amounting to 0.3 to 0.4 per cent. must be made to allow for the presence of insoluble matter (yeast) in the wash.A. G. L. Detection of Butter-Fat, Cocoanut Oil and Palm Oil in Cacao Butter. F. Strube. (Zeit. ofentl. Chem., 1508, 14, 67-70.)-The method employed was originally proposed by R. Cohn, and is based on the fact that the soap formed on saponifying cacao butter is quite insoluble in sodium chloride solution, whilst the soap obtained from cocoanut oil, etc., cannot be salted out completely from its aqueous solution, The method is applicable to the testing of the fat obtained from chocolates, etc. About 2.5 grams of the fat are saponified by heating withTHE ANALYST. 189 alcoholic potassium hydroxide solution, and the alcohol is evaporated on the water-bath. The residue of soap is dissolved in 55 C.C. of hot water, and, when the solution is cold, 50 C.C. of saturated sodium chloride solution are added.After the lapse of fifteen minutes, during which time the mixture is stirred frequently, the whole is poured on a filter, and to 60 C.C. of the filtrate a further quantity of 50 C.C. of the sodium chloride solution is added. I n the case of pure cacao butter the solution remains clear or exhibits only a faint turbidity ; the fat from (‘ milk chocolate ” also yields a clear solution, whilst cocoanut oil and palm oil give more or less heavy precipitates. If, after a short time, the solutions be again filtered and the filtrate acidified‘ with hydrochloric acid, the solution remains quite clear should the fat be cacao butter or the same mixed with butter-fat, whilst with cocoa- nut oil and palm oil a further turbidity is produced.The solution has also the characteristic odour of cocoanut oil fatty acids. The presence of butter-fat may be detected by the odour of butyric acid when the filtrate is acidified. I t is mentioned that the fat obtained from pressed and alkalised cocoas has the same melting-point and iodine value as pure cacao butter, showing that the treatment does not alter the composition of the fat, whether the alkali used be ammonia, potassium carbonate, or both. w. P. s. Estimation of Cocoanut Oil in Butter. G. R. Thompson and A. R. Tankard. (Chem. News, 1908, 97, 146.)-The authors have submitted the process described by T. R. Hodgson (ANALYST, 1908,49) to a critical examination, and find that the method is quite valueless for the estimation of cocoanut oil in butter.This conclusion is in agreement with that of Ross and Race (ibid., 1908, 122). The figures obtained in the experiments failed to differentiate butter from butter-substitutes or cocoanut oil. In the absence of any fatty acids, the sulphuric acid employed was found to have a, considerable action on the permanganate solution. w. P. s. Estimation of Mustard Oil. M. Kuntze. (A~chiv. Pharm., 1908, 246, 58-6Y.)--The following conditions are given for the volumetric estimation of mustard oil in alcoholic solutions of the same : Five C.C. of the tincture, containing about 2 per cent. of the oil, are placed in a 100 C.C. flask, 10 C.C. of ammonia and 50 C.C. of .& silver nitrate solution are added, the flask is attached to a reflux condenser, and its contents heated for one hour by means of a water-bath, which is kept boiling gently.After cooling, thc mixture is diluted with water to a volume of 100 C.C. and filtered. Fifty C.C. of the clear filtrate are then acidified with nitric acid, 1 C.C. of animonium ferric sulphate is added, and the excess of silver nitrate is titrated back with ;k ammonium thiocyanate solution. The author finds that a portion of the mustard oil is converted into allyloxythiourethane if an alcoholic solution of the oil be kept for a long time. This change may account for the untrustworthy results sometimes obtained on the analysis of old samples of the tincture. w. P. s. A New Vegetable Oil. P. Buttenberg. (Zeit. Untewich. Nahi.. Geizzissm., 1908, 15, 334-338.)-The author has recently examined an oil said to be obtained190 THE ANALYST.from the seeds of a Chinese plant; no particulars of the seeds are given, except that they are stated to resemble linseed. The oil had the following chemical and physical constants : Refraction at 40" C. ... ... ... ... ... 47.0 Acid value ... ... ... ... ... 9.4 Reichert-Meissl value.. . ... ... ... ... 34.8 Polenske value ... ... ... ... ... 0.5 Saponification value ... ... ... ... ... 234.7 Iodine value ... ... ... ... ... ... 64-6 Uneaponifiable matters ... ... ... . . . . 0.38 per cent. ... The oil gave a feeble reaction for sesame oil, but no reaction for cotton oil. Phytosterol acetate, melting at 180" C., was obtained from the unsaponifiable matters present in the oil. This melting-point is considerably higher than that of pure phytosterol acetate, and indicates the presence of dihydrophytosterol (ANALYST, 1907, 32, 424).w. P. s. Composition of Oil of Tarragon. M. Daufresne. (Bull. SOC. Chim., 1908, [iv. J 4, 330-335.)-0iI of tarragon (drtemisia draczmczdiu), which is largely used for flavouring condiments, consists of from 60 to 75 per cent. of estragol, 15 to 20 per cent. of tarpenes, and 0.5 to 0.6 of 23-methoxycinnamic aldehyde. Anethol is not present. The author has separated the terpenes into various portions, from which he has isolated an unsaturated substance analogous to myrcene and ocimene, and probably identical with the latter, and a cyclic hydrocarbon having dextro-rotary properties and closely resembling phellandrene. Two samples of the oil gave the following figures on examination : Specific gravity at 15" C.... ... ... Refractive index ,, ,, ... . . . Rotation at 20" C. ... Distilling under 1 4 mm. pressure at: 70" to 90" C. (Terpenes) ... ... 90" to 110' ,, (Estragol) .. ... 110" t o 160" ,, ... ... 160' to 180' ,, (Aldehydes) ... ... Residue, by difference ... .. ... ... 9 , ... ... French Oil. 0.949 1.517 + 7.8" German Oil. 0.945 1.5165 + 7.24" 17.6 grains 77.0 ,, 0.8 gram 1.2 grams 3.4 ,, w. P. s. Analysis of Oil of Lavender. P. Jeancard and C. Satie. (Bull. SOC. Chim., 1908, [iv.] 4,155-159.)-0f late years, owing to the increase in its price, there has been a hndency to adulterate oil of lavender, and the authors give certain limits within which, in their opinion, the chemical and physical'constants of oil of lavender ought to fall.The chief of these limits are : Specific gravity at 15" C., 0.880 to 0.890 ; rotation, - 6' to - 10" ; saponification value after acetylation, over 160. The figuresTHE ANALYST. 6.5 per Cent. Alcohol. 191 Before Acetylstion. are arrived at after the examination of a number of pure oils of lavender, the results of which analyses are given in the following table : LAVENDER FROM UPPER ALPS TO SUMMITS OF LOWER ALPS. -8.4" to t o - 9 " --6'to - 8.4" - i.1" to - 9.3" Yew. 1.7 2 t o 2.1 1.9 1905, 3 samples. 1906, 2 sninples. 1907, 4 samples. 2.6 t o 2.5 2.2 t o 2'6 3.0 t o 3'9 1906, 5 samples. 1906, 2 samples. 1907, 3 samples. 33.1 t o 65'1 65'1 t o 72'8 62.3 t o 8t.i Specific Qravity. 0.8854 tc 0 * 89 00 0.5872 t c 0.8580 0.8Si5ti to 0*5000 0.8828 to 0'8848 0.8836 t o 0.8848 0'8840 t o 0.8870 Rotation.- 7.10" LO -. 6.1" t o - 6.4" -;9 t o -- 8.3' - .L - 4 3olubility in Parts of- Saponification Value- 0 per Cent. Alcohol. 2 t o 2.7 2-4 to 2.5 2.3 t o 2.6 4.6 to 20 5.1 t o 20 20 91.7 t o 1 23 '9 100.1 t o 111 94 5 t o 131.6 I After icetyliition. 171 '5 to 179.9 166'6 t o 172.8 1;5 t o 194.5 16.5'9 t o 1 72.2 164-4 t o 167.2 170.9 to 188.3 Estcrs. 32 09 t o 43.36 35-05 to 38'85 33 07 to 46-06 20.33 to 22-79 25'46 t o 22.79 21'81 t o 29.64 The saponification value after acetylation is of importance, as it is a measure of the alcohols present in the oil. Adulteration with oil of spike-lavender increases the specific gravity and diminishes the saponification value, that of oil of spike-lavender Detection of Bilberry Juice in Red Wines.W. Plahl. (Zeit. Unterszcch. Nahr. Genussm., 1908, 15, 262-269.)-The reaction for bilberry juice, described previously (ANALYST, 1907, 32, 92), may be applied to the detection of this juice in completely fermented red wines. Fifty C.C. of the wine are rendered feebly alkaline in reaction by the addition of sodium hydroxide solution, and evaporated to a volume of about 25 C.C. After diluting to the original volume, the colouring matters of the wine are precipitated by the addition of lead acetate, and the mixture is filtered. A portion of the clear filtrate is treated with sodium sulphate, the lead sulphate is filtered off, the filtrate is acidified with hydrochloric acid, and heated on a, boiling water-bath. The blue coloration is obtained if the wine contains not less than 2 per cent. of bilberry juice. In some cases the colouring matters are not completely precipitated by lead acetate, and a faint red coloration may be produced on adding the hydrochloric aoid; this red coloration, however, appears at once (while the solution is cold), and the blue coloration, due to the bilberry juice, becomes visible being below 100. (See also ANALYST, 1900, 25, 297.) w. P. s. only when the solution has been heated for a little time. w. P. s.

 

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