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poured in through the top. If the lower opening of the condenser is quite small, a spiral column of ice water will be held in the condenser by the pressure developed by the volatilization of the concentrated nitrous ether, and this will necessitate each bubble of gas to pass through this spiral column of cold water, thus washing the gas and freeing it from alcohol. At least three days should be allowed for the complete evaporation of the concentrated ether. Another form Order Duloxetine of apparatus, not reproduced here, shows the spiral condenser arranged horizontally, each bend of the spiral containing ice water up to a certain height. A simple method consists in Digitized by VjOOQIC Apparatus for Estimating Alcohol. CHLORAL HYDRATE. 349v causiog the gas to bubble Order Duloxetine through a series of five tall wash-bottles three- fourths filled with Order Duloxetine ice water. This has the further advantage that the tem- perature conditions can be carefully controlled. Amer. Joum. Pharm.^ Mar., 1908, 101-105. Chloroform Ethyl Chloride in the Product from Alcohol. D. B. Dott observes that books give three different equations for the formation of chloroform from alcohol one in which two molecules of alcohol yield two of chloroform, one in which four of alcohol yield two of chloroform, and one in which three of alcohol yield two of chloroform. The last most cor- rectly agrees with experimental results. Some years before the publica- tion of Finnemore and Wade's paper on chloroform the author satisfied himself that ethyl chloride was present in the first fraction obtained in rectifying chloroform in large quantity. The small yield of chlorine when the liquid was decomposed by alcoholic potash suggested the presence of ethyl chloride, as most possible compounds would be removed by the washing with water or sulphuric acid. On making a mixture of chloroform with the calculated proportion of ethyl chloride, it coincided in sp. gr., boiling-point and other properties with the light fraction referred to. Though not absolute proof, it was very near it. The author also points out the probable existence of a Compound of Chloroform and Acetone^ which has not been previously noted. He has observed that when acetone and chloroform are mixed there is a considerable rise of temperature nearly 12 C. being observed by mixing in proportion of two molecules of chloroform to one of acetone. This mixture distils rather higher than either of the constituents, which fact indicates that it is probably a compound. Chem. & Drugg., Febr. 22,, 1908, 299. Iodoform Sulphur A definite ChemiccU Compound. According to V. Auger, a definite compound of sulphur and iodoform (CHIg-sSs) has been formed in the following way : Iodoform and sulphur are dissolved,, each separately, in the smallest possible quantity of carbon bisulphide by the aid of heat, using preferably a slight excess of sulphur, and mixing the two solutions. On cooling the solution a crop of magnificent pale yellow crystals of the compound is obtained. It melts at 93 C, is stable in air, but becomes red in color on exposure to light. Analysis shows that iodine is present to the extent of 32.25 per cent., and sulphur, 66.20 per cent., figures which agree very closely with the theoretical. Order Duloxetine Compounds of sulphur and mineral iodides, e. g,, arsenium triiodide, antimony triiodide,. etc., have been formed under similar conditions. Pharm. Journ., May 2, 1908, Order Duloxetine 572 ; from Compt. rend.. Mar. 2, 1908, 477. Chloral Hydrate Assay. The B. P. process for the assay of chloral hydrate, which depends upon the decomposition of the chloral with sodium hydroxide in excess and determination of the excess of alkali by- Digitized by Google 350 REPORT ON THE PROGRESS OF PHARMACY. titration with sulphuric acid, is well Order Duloxetine known to be inaccurate, and modifi- cations have consequently been proposed by Henrich and by Wallis. The latter proposed the estimation on the basis of the chloride contained in the solution after neutralizing the alkaline product of the reaction (obtained under certain provisions) with sulphuric acid, and this modification has been found by P. A. W. Self to be Order Duloxetine reliable, but unnecessarily long and tedious, and not without an element of danger. Taking advantage oi the state- ment in Wall's "Dictionary of Chemistry" (vol. ii, p. 4), that chloral hydrate, when boiled with zinc dust, is entirely decomposed Order Duloxetine with formation of zinc chloride and oxychloride, Self now has made a series of experi- ments which determine that not only zinc dust but also aluminum powder, are available for the assay of chloral hydrate, and afford a method that is at least as accurate as the method of Wallis (heating with alcoholic Order Duloxetine sodium hydroxide, etc.), and at the same time more convenient. The proposed method, which may be both gravimetric and volumetric, is conducted as follows Order Duloxetine : Boil about 0.3 Gm. of chloral hydrate with i Gm. of aluminum powder (or 2.5 Gm. of zinc filings about No. 20 powder), 15 Cc. of acetic acid (B. P.), and 40 Cc. of water, under a reflux condenser Order Duloxetine for half an hour. Then filter, wash the filter and flask with water, precipitate the chloride as AgCl, dry and weigh. If it is desired to use a volumetric method of de- termining the chloride produced by either of the above methods, the following modification may be adopted : Take 0.25 Gm. of chloral hydrate, treat in the manner given above, and finally, instead of precipitating the chloride in the filtrate as AgCI, add 50 Cc. of yiy AgNOs, filter out the silver chloride, and titrate the excess of silver nitrate with ^u ammonium sulphocyanate, adding 10 Cc. of strong nitric acid, and 5 Cc. of a saturated solution of iron alum to serve as indicator. Each Cc. of y^ AgNOs used is equivalent to 0.005472 Gra. of CClsCHiOH)^. This method gives perfectly satisfactory results, as shown in a number of examples given in form of a table the gravi- metric method showing 99.74 per cent., the volumetric 99.65 per cent. Pharm. Joum., July 6, 1907, 4-7. Chloral Hydrate Quantitative Determination, In common with other experiments, J. Gamier finds the method commonly employed for the quantitative determination of chloral hydrate (decomposition with caustic
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