P.

Joseph-Nathan I
y
Centro de lnvestigoci6n
de Estudios Avonzodos del I.P.N. 1 Liquid-Liquid EX~III~~~OII
Me'xico 14, D.F., Me'xico
I
Liquid-liquid extraction provides a good The distillation-extraction bead, b, and the condenser,
laboratory method for the separation of many organic c, are mounted. A boiling granule and 60 ml of
mixtures.' We would like to show how this can be cyclohexane are placed in the 100-ml round bottomed
done in a simple manner using commercially available flask, a, equipped with a heating mantle and a Variac
substances and an apparatus of small dimensions that operated a t 90 v. The apparatus is then assembled and
still allow the experiment to be followed visually. the operation is started. After 10 min the cyclohexane
The experiment is designed to introduce students to solution in flask a begins to turn blue, and 20 min later
laboratory techniques which are not usually taught in only a pale color remains in the ethanolic solution.
general chemistry courses. Finally, after a total time of 45 min, no azulene can be
The equipment used in the experiment is schematic- detected in the ethanolic solution even by scanning an
ally represented in the figure, and works as follows: ultraviolet spectrum.
The extracting solvent is placed in flask a, which is
heated. The vapors pass through the broad branch of
the distillation-extraction head, b, to the condenser,
c; the condeusate drips through a tube to the bottom of
flask d, in which the solution to be extraced is placed.
Since the density of the extracting liquid is lower than
that of the solution, it flows to the surface, extracting
part of the solute during its ascendent course through
the solution. When the level of the extracting liquid
reaches the narrower branch of the extraction head,
b, it begins to return to flask a where the extracted
compound accumulates progressively. I n this way a
constant flow of fresh extracting solvent passes through
the solution placed in flask d.
I n order to follow easily the course of the experi-
ment, we have chosen a system with a nearly ideal
behavior, since the solubilities and, therefore, the
partition coefficient of the compound to he extracted
favor the extracting liquid much more than the solvent
in which it is initially dissolved.
The experiment is carried out as follows: a solution
of 5 mg of azulene (Aldrich Chemical Co.) in 7 ml of
ethanol is diluted with 3 ml of distilled water, and the
resulting blue liauid transferred t o the 25-ml flask d.
' CRAIG,L. C., AND CRAIG, D., "Technique of Organic Chem-
istry," (Edilor: WEISSBERGER, ARNOLD),Vol. 111, Interscience
Publishers (division of John Wiley & Sons, Inc.), New York,
1950. Apporobr for liquid-liquid extraction

176 / Journol of Chemical Education