EXPERIMENT 3

DETERMINATION OF THE DISTRIBUTION OF ACETIC ACID BETWEEN WATER

AND BUTANOL IN A MIXTURE IN THE TWO-PHASE REGION OF A TERNARY
PHASE DIAGRAM

OBJECTIVES:
At the end pf this exercise, the students should be able to:
1. Determine the composition of the conjugate solutions using titration.
2. Draw the tie lines and determine the delta point and plait in the ternary phase diagram.
3. Determine the amount of acetic acid in the water-rich phase and butanol-rich phase in a mixture
in the two-phase region of a ternary diagram using the lever rule.

INTRODUCTION:
Acetic acid is an organic compound that is most widely used carboxylic acids in many reactions
and as solvents. It is an important laboratory reagent and solvent for carrying reaction since it remains
fixed or constant by oxidizing and reducing agents. And in organic chemistry, I is important to determine
how much of an organic compound is dissolved in an aqueous solution phase or vice versa because
sometimes it is deemed necessary to know the mutual solubilities of liquids in a two phase system and
one component may affect different synthetic routes. Therefore, a ternary phase diagram can be a tool to
calculate the mutual solubilities of liquids in a two phase region. As shown in figure 3.1, point a in the
region of immiscibility has an upper layer with composition equal to point c and a lower layer with
composition equal to point b. connecting point c and point b results in a tie line.
In this experiment, the composition of the aqueous layer and the butanol layer of a certain
solution in the region of immiscibility will be determined using the composition of the intersection of the
tie lines with the phase boundary. Tie lines are the slanted lines that intercepts on the curved line of a
region in a phase diagram where two phases exists. These lines are needed to find the composition of the
individual phases in a two-phase region. The tie lines are
created by connecting the composition of the upper and
lower layer of the two-phase mixture.
Once the composition of the two phases is known, the
determination for how much of each phase exists can be
found by using the lever rule.
In terms of mole fraction:
In terms of mass fraction:
Where nc is the moles of component C, n b is the moles of
component B, mc and mb are the mass of component C and B,
respectively, and ab and ac are the length of the segments ab and ac, respectively.
Tie lines that are created using different points and are extended to a certain point outside the ternary
diagram is called the delta point. It is a very vital in guessing the compositions of the upper and lower
layers of a certain point in the two-phase region. The delta point is also used in finding the Plait point.
The Plait point is the point which the compositions of the two-phases in equilibrium become equal and is
not located at the maximum of the curve since tie line are not horizontal.

METHODOLOGY:

List of Chemicals/Materials:
-

water
butanol
acetic acid
technical grade acetone

List of Apparatus and Set-up:

-

Erlenmeyer Flask (250mL)

Pipette and aspirator
Separatory Funnel and holder
Pycnometer
Beakers (100mL)
Burette and burette holder
Pipette (10mL)
Parafilm

Procedure:
Note: Use the ternary diagram determined in Experiment 2.
A. Preparation of Mixtures

A-BC
100
-

Compositions must be within the

two phase region in the ternary
diagram and will equal volumes
of conjugate phases.

Separatory
Funnel
-

Equilibriate at 25C
Separate conjugate phases

Cover and Label mixtures

properly.
Repeat until 4 mixtures are

Erlenmeyer
Flask

B. Measurement of Density

1
-

Transfer the conjugate phases.

Pycnomet
er
-

Weigh Pycnometer: empty, with

water, and with conjugate
phases.

END
C. Titration

1
5 mL
PHENOLPTHAL
EIN

Erlenmeyer
Flask

1.0 M NaOH
-

Titrate until phenolphthalein

endpoint.
Calculate % w/w CH3COOH in
each of the conjugate phases

END

References:
http://penerbit.uthm.edu.my/ojs/index.php/JST/article/viewFile/655/600

https://www.csun.edu/~jeloranta/CHEM355L/experiment5.pdf
http://nptel.ac.in/courses/113106032/9%20-%20Phase%20diagrams.pdf
https://www.southampton.ac.uk/~pasr1/tielines.htm