METALLURGICAL ENGINEERING 18

Metallurgical Thermodynamics Laboratory

IMMISCIBLE SOLVENTS
Distribution of a Solute between Immiscible Solvents
I.

PRELAB QUESTIONS
1. What is distribution coefficient and what are the factors affecting it?
2. Starting from the thermodynamic equation of the chemical potential, derive the general formula for the
distribution coefficient. Assume total dependence on concentration.
3. Draw the chemical structures of ether, HOAc, and CCl 4. What can you infer about the solubility of the
solute with the solvents (read the procedure below)?
4. Draw a schematic diagram of a separatory funnel and briefly explain how it works. How is the bottom
layer extracted? How about the upper layer?
5. In step 2 of the procedure, it is noted that venting of gasses should be done regularly. Why should there
be expected buildup of gases?
6. In the solution preparation procedure, three 50-ml samples are to be prepared. Draft a procedure on
how you can produce these three samples with only one prepared sample and subsequent dilution.
Include calculations.

II.

MATERIALS
100-mL separatory funnels
100-mL Erlenmeyer flasks
100-mL volumetric flask
25-mL pipette
10-mL pipette

III.

1.0 N acetic acid or glacial acetic acid

0.5 N NaOH
0.01 N NaOH
Carbon tetrachloride (CCl4)
Ether

PROCEDURE1
1. 50-mL each of approximately 0.5 N, 1 N and 2 N solutions of HOAc in water is prepared. 25 mL of
each of the three solutions is pipette into closed 100-mL separatory funnels, and to each is added 25
mL of diethyl ether.
2. Vigorously shake the separatory funnel for around 30 seconds. Continue to shake it in a more
controlled manner for a good 15 mins, thereafter.
IMPORTANT: Frequently vent out gas buildup by removing the stopper.
3. Allow the solutions to come to equilibrium for an appropriate amount of time. There should be a clear
line between the two layers. No gas bubbles should be observable.
4. Rapidly drain 10-mL aliquots of each of the lower layers into Erlenmeyer flasks for titration with NaOH
(0.5 N) using phenolphthalein as indicator.
5. Aliquots (10-ml) of the upper layers are removed from the separatory funnel using 10-mL pipettes,
taking care not to take up any of the lower layer. Titrate with NaOH (0.5N) with phenolphthalein as
indicator, also.
6. A second set of experiments is carried out in the same way, this time using carbon tetrachloride (CCl4)
instead of ether.
IMPORTANT: It should be noted that the rapid titration of the CCl4 layer is done due to its rapid
evaporation on exposure to air. Titrate CCl4 layer with 0.01 N NaOH instead of 0.5 N.

IV.

GUIDE KEYWORDS2
Distribution coefficient.
Sources of error.

log C A

vs.

log C A

plot. n and unity. Applications. Recommendations.

subject to change as necessary

for RDR; take note however that in no way should your discussion be limited on these alone as these are only guide keywords to help your train of
thought; exercise scientific freedom and creativity
2