946
E. J . MCDONALD, A. F. KLUENDER AND R. W. LANE
THE SYSTEM ETHYL ALCOHOLGLYCEROL-CARBON TETRACHLORIDE AT 25OC. H. J. McDONALD, A. F. KLUENDER,'
AND
R. W. LANE'
Department of Chemistry, Illinois Institute of Technology, Chicago, Illinois Received Augvst 10, lo@?
The effect of a third component, carbon tetrachloride, on the separation of the pure substances from mixtures of glycerol and ethyl alcohol is of interest to the chemist and the chemical engineer. Knowledge of the solubility relationships of the system ethyl alcohol-glycerol-carbon tetrachloride is necessary in consideration of the feasibility of such a process. A review of the literature failed to reveal that data on this system had been published. As a preliminary step in the study of the system, the region of immiscibility and the tie-lie relationships have been determined. MATERIALS
The glycerol used was a specially prepared sample with a glycerol content of 99.8 per cent. It w&s obtained from the Armour Soap Works of Armour and Company, Chicago, through the courtesy of Mr. E. W. Colt, Chief Chemist. The alcohol used was the 200-proof material sold by Commercial Solvents Corporation. The carbon tetrachloride was of the best grade obtainable from the Eastman Kodak Company, and was used without further purification. PROCEDURE AND RESULTS
The procedure described by McDonald (1) for the system ethyl alcoholglycerol-benzene was used for determination of the region of immiscibility and the tie-line relationships of this system. The titrations were conducted a t 25.0 C. f 0.1' in small glass-stoppered bottles in an all-glass water bath. In the middle portion of the curve, ethyl alcohol was added until cloudiness disappeared. A foamy condition developed a t the end point, which facilitated its identification. At the extremities of the curve, careful observation was necessary after each addition to determine if any immiscibleportion was present. The property of cloudiness could not be used as an indication of immiscibility. At the carbon tetrachloride end of the immiscibility curve the mixtures, when shaken, tended to cling to the inside of the bottle as if the glass surface were waxed, but when the immiscibility was dispelled, the mixtures broke away cleanly from the glass. All samples were centrifuged at 25OC. as a check on whether the solutions were really homogeneous at the end point of the titration. Refractive-index, surface-tension, or density measurements, as means of determining the distribution of ethyl alcohol between glycerol and carbon 1
3
Present address: Victor Chemical Works, Chicago Heights, Illinois. Present address: National Aluminate Corporation, Chicago, Illinois.
SYSTEM ETHYL ALCOHOL-GLYCEROL-CARBON
TETRACHLORIDE
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TABLE 1 Solubilities at b6.OoC.
1
CAPBON TETPACBLORIDE
CLYCEPOL
CAPBON TETPACHLOPIDE
weighl Per ccnl
weigh1 )