Toxicological analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1899)
卷期: Volume 24, issue 1  

页码: 11-13

 

ISSN:0003-2654

 

年代: 1899

 

DOI:10.1039/AN8992400011

 

出版商: RSC

 

数据来源: RSC

 

摘要:

THE. ANALYST. 11 TOXICOLOGICAL ANALYSIS. Piutti’s Reagent for Alkaloids (Iodine-derivative of Para-ethoxyphenyl- succinimide). G. Simoncelli and N. Scarpitti. (Gaxx. chim. Ital., 1898, xxviii. 1121, 171 ; through Chem. Zeit. Rep., 1898, 279.)-The authors have investigated several iodine reagents for alkaloids, including those of Bouchardat and Selmi, and they find the most delicate to be one of the substances recommended by Piutti- viz., the iodine derivative of p-ethoxyphenylsuccinimide. This is prepared by treating the h i d e with a solution of iodine and potassium iodide in acetic acid. F. H. L. Detection of Acatylene in Cases of Poisoning therewith. D. Vitali. (Boll. chim. farm. , 1898, xxxvii., 449 ; through C7zem. Zeit. Rep., 1898, 247.) -The suspected blood is mixed with 5 or 8 per cent.of pure acetone, placed in a retort, and distilled into an empty condenser and a set of absorbing bulbs containing more acetone. The retort is heated on a water-bath, the condenser and bulbs kept cold in ice. The acetone passes over, carrying the acetylene with it, and the latter may be identified by its characteristic reactions. Hydrogen sulphide and phosphide, which often occur in the crude gas, also dissolve in the acetone, and can be sought for therein. F. H. L. - . - -~ ~- Detection of Free Nitric Acid in Toxicological Work. D. Vitali. (Oester- reich. Chem. Zeit., 1898, 333.)-The organs to be examined are warmed on a water- bath, water being added if needful, and freshly precipitated barium carbonate is intro- duced, a little at a time, as long as it dissolves.The mixture is then evaporated to dryness, and the residue boiled three or four times with an equal volume of absolute alcohol. By this procedure the calcium and magnesium nitrates are brought into solution, whilst sodium nitrate, the calcium nitrate naturally present in the organism, and the barium nitrate formed by the action of the free nitric acid upon the barium carbonate, remain in the residue. The alcoholic solutions are then evaporated to dryness, the residue taken up with water and neutralized very carefully with solution of barium hydrate. The fluid is then again evaporated to dryness, and treated with absolute alcohol. The undissolved residue is taken up with water, the solution treated with a little lead acetate, to precipitate organic matter, and filtered.The filtrate is then treated with hydrogen sulphide, to remove the lead, filtered, and the clear filtrate concentrated by evaporation, and dried in an exsiccator. The residue is examined for crystals of barium nitrate, which can be recognised by their crystalline form and by the usual tests. In this way it is possible to determine those nitric acid12 THE ANALYBT. compounds with albuminous bodies (acidalbumins) which are soluble in alcohol, The insoluble residue from the first treatment with alcohol contains, as already mentioned, the sodium nitrate, the barium nitrate resulting from the treatment with barium carbonate, and the calcium nitrate which must be regarded as a normal con- stituent of the body. I t is made slightly alkaline with sodium carbonate, by which the nitric acid of the acidalbumins insoluble in absolute alcohol is neutralized, and the barium nitrate resulting from the free nitric acid is converted into sodium nitrate, whilst the calcium and sodium nitrates remain unchanged.The solution is filtered, the filtrate evaporated to dryness, and the residue treated with boiling absolute alcohol, which takes up the calcium nitrate, whilst leaving the sodium nitrate undissolved. The insoluble portion is dissolved in water, treated with a slight excess of lead acetate, the solction filtered, and the lead separated by hydrogen sulphide. The clear colourless fluid which is thus obtained is concentrated by evaporation, and dried in an exsiccator. Crystals of sodium nitrate in this residue can then be detected by the usual tests.Another method which the author has used successfully is as follows: The intestines are cut into small pieces, and treated with freshly precipitated strychnine. As strychnine nitrate has an acid reaction, the neutralization cannot be controlled by means of litmus paper, The mixture is dialyzed, the residue twice extracted with warm water, the filtered fluids evaporated to dryness, and the residue treated with boiling alcohol. The alcoholic solution is then filtered, evaporated to dryness, the residue taken up with water, decolorized by treatment with lead acetate, followed by hydrogen sulphide, and the filtrate concentrated. Strychnine nitrate, formed by the union of the strychnine with free nitric acid, if present, would here crystallize out, and be determinable in the usual way.H. H. B. S. Destruction of Organic Substances in Chemico-Forensic Work. C. Kippen- berger. (Zeit. fiir Untemuclz. de.i Nahr. m d Genussmittel, 1898, 683-687.)-Villiers a short time since (Conzpt. Rend., 1897, 1457) advised the use of a mixture of nitric and hydrochloric acids, with the addition of a solution of a manganese salt, for the destruction of organic substances. He stated that with this mixture the liver, spleen, and lungs could be oxidized in a few minutes, and the muscles within an hour-much more quickly, in fact, than by the use of potassium chlorate and hydrochloric acid, as recommended by Fresenius and Von Babo. The author is unable to confirm this, but found, on the contrary, that in order to complete the action it became necessary to add potassium chlorate from time to time with continued heating. The experiments made with Villiers’ method, however, led to the trial of a manganese salt in con- junction with potassium chlorate and hydrochloric acid, and in this case the author found a decided acceleration of oxidation to result from the use of manganese. The most suitable manganese compounds for the purpose are manganic dioxide and manganous chloride, of which the former has the advantage of being a stock reagent in every laboratory. The sulphate is less suitable, on account of the possibility of metals in the case of metallic poisoning (e.g., lead, mercury, or silver) becomingTHE ANALYST. 13 converted into insoluble sulphates, and so causing difficulties in the subsequent analysis. It is sufficient to add a little manganic dioxide to the substance mixed with hydrochloric acid, and then to follow up with potassium chlorate in the usual way. H. €€ B. S.

 

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