LABORATORY EXPERIENCE: Liquid-Liquid Extraction (Functional Design)

This laboratory demonstration aims at creating the triangular diagram of a water-THF-

cyclohexane mixture to determine which thermodynamical model better adjusts to the
collected data.

To determine a system such as the presented one, the binodal curve and the tie lines must be
found. The binodal curve separates the region with one phase from the one with two phases. In
the region where two phases coexist, the tie lines determine the composition of the two phases
formed. Cloud points are the points which define the binodal curve, and its main characteristic
is that turbulence can be observed in the solution. This is used to determine the points in the
binodal curve.

Your goal: Draw the triangular diagram of a water-THF-cyclohexane mixture at room

temperature and determine the composition of a binary mixture to be extracted.

Some of the questions to answer are:

a) What is liquid-liquid extraction? List the solutions or streams involved in a liquid-liquid

extraction operation.
b) What are binodal curves? What are tie lines? What is a cloud point?

Your specific objectives:

a) Determine the binodal curves of the samples.

b) Determine the tie lines.
c) Determine the composition of the binary mixture to be extracted.

Experimental procedure:

The procedure employed to determine the binodal curve consists of preparing solutions of
solute and inert or solute and solvent, of known concentration, and add the third component
until the solution becomes turbid (cloud point). This is the stability limit of the ternary mixture.
In 100 mL Erlenmeyers, prepare four binary solutions of solute and inert (for the side rich in
inert), and four binary solutions of solute and solvent (for the side rich in solvent). The addition
of the third component is done with a burette, slowly. However, the precision of the burette is
not enough, so the amount of solvent/inert added must be calculated weighting the sample
after the addition. These solutions are also used to prepare a calibration curve, by measuring
the refractive index for the solutions of known concentrations.
To determine the tie lines, three ternary mixtures of known composition (under the binodal
curve) are prepared. These solutions are unstable and will separate in two phases. When the
two phases are separated, samples are collected from both solutions and the refractive index is
measured, to determine the content of THF in each fraction.

MEQ – FUNCTIONAL DESIGN LABORATORY | L-L Extraction

Approximate values for the preparation of the mixtures:
Binodal curve:
PTHF (g) PH2O (g) PCH (g)
1 13.1433 36.5523 0.007
2 25.1098 24.1642 0.1826
3 33.0486 15.5010 0.8627
4 38.7894 8.8747 1.6822
5 17.1936 0.1817 32.4926
6 29.5929 0.5825 19.4282
7 38.1010 1.7339 10.0561
8 40.4993 2.9571 6.1037
Tie lines:
PTHF (g) PH2O (g) PCH (g)
9 2.5270 8.3483 7.0385
10 6.4537 7.6148 3.8547
11 9.8874 6.9674 1.0668

Safety rules and recommendations:

➢ Whenever possible, work under the extraction cabinet.
➢ Use the analytical scale to measure the amount of liquid added with the burette.

Planning:

Day 1 Day 2 Day 3 Day 4

Answer the preliminary questions in the report
Determine the binodal curve from the water-rich solutions
Determine the binodal curve from the cyclohexane-rich solutions
Determine the tie lines
Determine the compositions for the binary mixture to be extracted

References:

1. McCabe, Warren L. (Warren Lee), 1899-1982. (2001). Unit operations of chemical

engineering. Boston :McGraw Hill. Section 4. Chapter 20. Leaching and extraction.
2. Amrit N. Patel. (1983) Ternary Phase Equilibrium Studies of the Systems
Tetrahydrofuran-Water-Solvents. J. Chem. Tech. Biotechnol. (33A). 245-248.
https://doi.org/10.1002/jctb.504330505

MEQ – FUNCTIONAL DESIGN LABORATORY | L-L Extraction