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Turla N. (Ternary Liquid Experiments)

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TURLA, NYGEN KEITH LOUISE D. (18-05544)
BS Chemical Engineering
PHYSICAL CHEMISTRY FOR ENGINEERS 2
ACTIVITY 1
LABORATORY EXPERIMENTAL PROCEDURE FOR A TERNARY LIQUID SYSTEM
MISCIBILITY GAP IN A TERNARY SYSTEM
Overview
Short description
Principle
A number of completely miscible two component mixtures are prepared to investigate the
three component acetic acid / chloroform / water system. These mixtures are titrated with the
third component until a two phase system is formed which causes turbidity. The phase
diagram for the three component system is plotted in a triangular diagram.
1
TASKS
1. Titrate nine different acetic acid / chloroform mixtures with water until a two phase
system is formed in each case.
2. Titrate six acetic acid / water mixtures with chloroform until phase separation is
observed.
3. Plot the results of the titrations, expressed as molar fractions, in a trianglular
diagram.
PROCEDURE
1. Set up the experiment as shown in Fig. 1.
2. Prepare the chloroform / acetic acid mixtures listed in Table 1 by weighing the
specified quantities of chloroform and pure acetic acid into 100 ml flat-bottomed
flasks.
Table 1: Quantities and mixing proportions of chloroform / acetic acid mixtures
MIXTURE
mchloroform (in g)
nchloroform
macetic acid (in g)
nacetic acid
A
119.5
1.0
0.0
0.0
B
107.6
0.9
6.0
0.1
C
95.6
0.8
12.0
0.2
D
83.7
0.7
18.0
0.3
E
71.7
0.6
24.0
0.4
F
59.8
0.5
30.0
0.5
G
47.8
0.4
36.0
0.6
H
35.9
0.3
42.0
0.7
I
0.0
0.0
60.0
1.0
3. Shake the samples well and transfer 10 g of each mixture to suitably labelled test
tubes.
4. Temperature equilibrate the test tubes to 25 °C in a temperature controlled water
bath.
5. Titrate the samples with distilled water from a microburette until the liquid becomes
turbid as a result of separation.
6. Shake the test tubes from time to time to ensure good mixing of the samples (insert
rubber stoppers before shaking).
7. Record the quantity of water added (in ml) as approximation for the mass of water (in
g).
8. Repeat the procedure for samples K to P listed in Table 2.
Table 2: Mixing proportions of water/acetic acid
MIXTURE
mwater (in g)
nwater
K
1.00
9.00
L
2.00
8.00
M
3.00
7.00
N
4.00
6.00
O
5.00
5.00
P
6.00
4.00
macetic acid (in g)
10
20
30
40
50
60
nacetic acid
0.021
0.046
0.076
0.113
0.161
0.22
9. Again transfer 10 g of each sample to a separate test tube and temperature
equilibrate them to 25 °C in the temperature controlled bath.
10. Titrate with chloroform until turbidity occurs and record the quantity added.
11. Calculate the mass of chloroform from the density ( ρchloroform= 1.489 g / ml) and the
consumption (in ml).
12. Calculate the molar fractions for all mixtures and plot the results in a phase diagram
using triangular co-ordinates (see Fig. 2)
2
Source: https://repository.curriculab.net/files/versuchsanleitungen/p3030601/p3030601e.pdf
3
ACTIVITY 2
EXAMPLES OF THE TYPES OF PARTIALLY MISCIBLE THREE-LIQUID SYSTEMS
TYPE 1 FORMATION OF ONE PARTIALLY MISCIBLE PAIR
Mixture 1 Acetone-Water-Methyl isobutyl ketone
MISCIBLE
Acetone-water
Acetone-methyl isobutyl ketone
Mixture 2 Methanol-water-chloroform
MISCIBLE
Methanol-water
Methanol-chloroform
Mixture 3 water-benzene-alcohol
MISCIBLE
Water-alcohol
Benzene-alcohol
Mixture 4 Acetic acid-chloroform-water
MISCIBLE
Acetic acid-chloroform
Acetic acid-water
Mixture 5 Acetone-water-phenol
MISCIBLE
Acetone-water
acetone-phenol
PARTIALLY MISCIBLE
Water-methyl isobutyl ketone
PARTIALLY MISCIBLE
Water-chloroform
PARTIALLY MISCIBLE
Water-benzene
PARTIALLY MISCIBLE
chloroform-water
PARTIALLY MISCIBLE
water-phenol
TYPE 2 FLORMATION OF TWO PARTIALLY MISCIBLE PAIRS
Mixture 1 Aniline-n heptane- methylcyclohexane
MISCIBLE
n heptane-methylcyclohexane
Mixture 2 Nitrile-water-ethanol
MISCIBLE
water-ethanol
Mixture 3 Water-phenol-aniline
MISCIBLE
phenol-aniline
Mixture 4 Water-ethyl acetate-n butyl alcohol
MISCIBLE
ethyl acetate-n butyl alcohol
PARTIALLY MISCIBLE
Aniline-n heptane
Aniline-methylcyclohexane
PARTIALLY MISCIBLE
Nitrile-water
Nitrile- ethanol
PARTIALLY MISCIBLE
Water-phenol
Water-aniline
PARTIALLY MISCIBLE
Water-ethyl acetate
Water-n butyl alcohol
4
Mixture 5 Methanol-water-heptane
MISCIBLE
Methanol-water
PARTIALLY MISCIBLE
Water-heptane
Methanol-heptane
TYPE 3 FORMATION OF THREE PARTIALLY MISCIBLE PAIRS
Mixture 1 Succinic nitrile-water-ether
MISCIBLE
PARTIALLY MISCIBLE
Succinic nitrile-water
Succinic nitrile-ether
water-ether
5
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