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Q2015 Physical Chemistry Measurements Laboratory

Chemistry Department, Campus Monterrey


Practice # 8
Distribution Coefficient
CONTENT:

Distribution equilibrium of immiscible phases


Concepts in the purification of substances by liquid-liquid extraction

OBJECTIVES
In this experiment, you will

Determine the distribution coefficient (K), in a system of two immiscible liquids


Learn the importance of the concept of distribution, purification of substances by liquidliquid extraction.

PRE PRACTICE ACTIVITIES

Remember basic knowledge of heterogeneous equilibrium

INTRODUCTION
If a mixture of two immiscible liquids an excess of a liquid or a solid is added, this will be
distributed between the two phases, so that each reach the point of saturation. When the
substance is added to the two immiscible solvents, in sufficient quantity to saturate, that will be
distributed between the two layers in a given ratio of concentrations.
In a system of two immiscible liquids, a dissolved substance is distributed between the two liquids
according to a defined balance called distribution coefficient (K).
If a solute associated exists in a phase (a) and dissociated in a phase (b) have the equation 1.
According to the principle of chemical equilibrium, the system will be in equilibrium when the
chemical potential of the solute in (a) and (b) are equal, equation 1:
(1)

When;

(2)

Were represents the standard chemical potential, the activity coefficient and C is
concentration.
Substituting in the equation we obtain:

If and are the concentrations of the substance in a and b, at constant temperature and
considering that
we obtain equation 3:
(3)
This relationship is applied when the solute is completely associated or dissociated. When de
association or dissociation is partial, its necessary to apply a more rigorous derivation.

Fig. 1 Equilibrium made by the benzoic acid in the aqueous phase and in the organic phase.

MATERIALS
4 Ring stand

1 burette clamp

1 50ml Burette

3 3finger clamps

3 150mlSeparation funnel

1 2ml volumetric pipette

6 125ml Erlenmeyer flasks

1 5ml volumetric pipettes

1 1L beaker

1 25ml graduated cylinder

3 small rings

3 100ml beakers

1 heating grill

Face mask

PROCEDURE
Verify with your team that your given material is complete and good.
Before you start the experiment make sure you have all the necessary substances to work
correctly.

1. CO2-free water is prepared by boiling vigorously for 10 min distilled water contained in a
beaker of 1 liter. Allow to cool without air access.
2. 25ml of CO2-free water and 25 ml of toluene are placed in each separation funnel. These
are numbered and are added 1.1; 1.5 and 1.9 g of benzoic acid to each, see Figure 2.

Fig. 2 Separation funnels with mixture

3. Close the funnels with the glass stopper and stir for 15 min. We recommend you handle
the funnel by the neck and the stem so that the mixture doesnt get hot by your hands.
After stirring a few minutes, invert the funnel and turn on the key occasionally, to avoid
increasing the internal pressure and prevent the mixture from spilling.
4. Place the funnel in the ring and allowed the mixture to separate into two layers perfectly
clear.
5. Take 2 ml of the organic layer of the first funnel and transfer to a 125ml erlenmeyer flask,
add 25ml of CO2-free water and a drop of phenolphthalein. The flask must be held with
clamps. The mixture is boiled on the grill and titrated with a standardized solution of
sodium hydroxide 0.025 M.
6. The same operation is repeated with the funnels No. 2 and No. 3.
7. Empty the aqueous part in three beakers (previously numbered). 5ml samples of each of
the vessels were taken and analyzed as above.
All titrations were done in duplicate. Assume that the two liquids are completely immiscible.
DATA ANALYSIS
Then the guide presents calculations to determine the distribution coefficient of an organic
sample. This guide tells you the different operations you perform to get your results.
You should use it as support to create your own format and perform all the transactions to get
your result.
Distribution Coefficient = K
1. Determine the solution molarities
a) Aqueous phase

Aqueous Phase
Flask 1
Flask 2
Flask 3

NaOH Volume

b) Organic phase

Organic Phase
Flask 1
Flask 2
Flask 3

NaOH Volume

= Benzoic acid concentration in toluene, moles/liter


= Benzoic acid concentration in water, moles/liter
Flask
1
2
3

log

log

2. Graph log Ca vs Log Cb, and calculate n from the slope in the graph.
3. With the obtained valuo of n, determine the distribution coefficient K.
a) Explain the meaning of n.
b) Determine the error rate in K.
% error rate=

The original table must be included in the report.

BIBLIOGRAPHY
1)Urquiza, M. Experimentos de Fisicoqumica Limusa-Wiley, Mxico, D.F. 1995
2) Visscher, F; Gaakeer, W.A; Granados P. J. Chem. Eng. Data 2011, 56, 3630-3636