UNIVERSITI SAINS MALAYSIA

SCHOOL OF CHEMICAL ENGINEERING

SEM 2, 2021/2022

EKC 291 – CHEMICAL ENGINEERING LABORATORY 1

EXPERIMENT 13: EQUILATERAL-TRIANGLE DIAGRAM
LAB REPORT

GROUP NUMBER : 25

GROUP MEMBERS : MAH HIN MAN 148703

TEOH YEE XUAN 152729
NURUL SYAFIQAH BINTI ARIFF 150134

INSTRUCTOR : PROF. MADYA DR. TYE CHING THIAN

TECH. IN CHARGE : NOR ASWANI MUHAMAD

DATE OF EXPERIMENT : 5/4/2022

DATE OF SUBMISSION : 11/4/2022

Table of Contents
Content Page

1.0 Abstract 1

2.0 Objective 1

3.0 Result 2

4.0 Discussion 5

5.0 Error Analysis 5

6.0 Conclusion 6

7.0 Reference 7

8.0 Appendix 8
1.0 Abstract
In this experiment, a research about liquid-liquid extraction involving ternary system
was made. The Equilateral Triangle Diagram proposed by Hunter and Nash is used for
the multistage extraction calculations for ternary system. The ternary diagram is the
main principle underlying estimating the number of phases required in a liquid-liquid
extraction process. The liquid-liquid extraction concept, for example, is used in the
wastewater treatment industry to remove dangerous chemicals like phenol from water
(Sas, Domínguez, González and Domínguez, 2018). The number of theoretical phases
necessary for efficient extraction can be visually determined and estimated in terms of
cost.
The three components used in this experiment are acetone, toluene and water
where the solute is acetone, the solvent is toluene, and the diluent is water. For both
toluene-rich phase and water-rich phase, the binodal curve are obtained in Experiment
1A and 1B via cloud point titration, then Experiment 2 is conducted to determine the tie
lines connecting the binodal curve. Based upon the results of Experiment 1A, by using a
best fit line it is found that the refractive index decreases linearly with increasing
acetone weight percent. It can be seen that for Experiment 1B, the refractive index
increases as the weight percent of acetone increases. The refractive index was measured
by using the refractometer and the corresponding weight percentage of acetone in
Experiment 2 were calculated by using the equations formed in Experiment 1
(calibration curve).

2.0 Objectives
The first objective of conducting these experiments is to obtain the binodal/solubility
curve for both water and toluene rich phases using cloud-point titration. Then, through
the experiments conducted, we are to determine the tie lines connecting the binodal
curves obtained in the experiments.

1
3.0 Results
Experiment 1A – Toluene Rich Phase
Table 1: Results for Experiment 1A (Toluene Rich Phase)

Volume (ml) Weight (g) % Weight Refractive Index

No.
Toluene Water Acetone Toluene Water Acetone Acetone Toluene 1 2 3 Average
1. 97.0 5.5 19.0 83.6431 5.4836 14.9036 14.33 80.40 1.47947 1.47942 1.48013 1.47967
2. 92.0 5 26.0 79.3316 4.9851 20.3944 19.48 75.76 1.47358 1.4735 1.47352 1.47353
3. 67.0 3.4 51.0 57.7741 3.3899 40.0044 39.54 57.11 1.39221 1.39218 1.39222 1.39220
4. 53.0 3.1 64.0 45.7019 3.0908 50.2016 50.71 46.17 1.35877 1.35881 1.35889 1.35882
5. 39.0 6.9 77.0 33.6297 6.8794 60.3988 59.86 33.33 1.36401 1.36493 1.36501 1.36465
6. 30.0 10.8 82.0 25.8690 10.7678 64.3208 63.71 25.62 1.36629 1.36593 1.36574 1.36599

Experiment 1B – Water Rich Phase

Table 2: Results for Experiment 1B (Water Rich Phase)

Volume (ml) Weight (g) % Weight Refractive Index

No.
Toluene Water Acetone Toluene Water Acetone Acetone Toluene 1 2 3 Average
1. 18.8 20.0 83.0 16.2112 65.1052 19.9404 64.30 16.01 1.37129 1.37122 1.37120 1.37124
2. 13.5 29.4 79.0 11.6411 61.9676 29.3124 60.21 11.31 1.36890 1.36908 1.36893 1.36897
3. 7.8 36.0 74.0 6.7259 58.0456 35.8927 57.66 6.68 1.36821 1.36818 1.36827 1.36822
4. 3.7 47.0 64.0 3.1905 50.2016 46.8599 50.08 3.18 1.36420 1.36418 1.36420 1.36419
5. 1.5 58.0 51.0 1.2935 40.0044 57.8272 40.36 1.30 1.35836 1.35867 1.35847 1.35850
6. 0.9 79.0 26.0 0.7761 20.3944 78.7646 20.41 0.78 1.34492 1.34566 1.34501 1.34520
2
Figure 1: Graph of Refractive Index against Weight of Acetone Figure 2: Graph of Refractive Index against Weight of Acetone

for Toluene Rich Phase for Water Rich Phase

Experiment 2 – Determination of Equilibrium Solute Distribution (Tie Lines)

Table 3: Result obtained from Experiment 2

Heavy Phase (Water rich) Light Phase (Toluene rich)

Volume (ml) Refractive Index %Weight Refractive Index %Weight

No.
(Acetone) (Acetone)
Toluene Water Acetone 1 2 Average 1 2 Average
1 21 20 76.5 1.36080 1.36188 1.36134 44.90 1.36663 1.36699 1.36681 56.61
2 30.5 20 69 1.35719 1.35523 1.35621 36.35 1.36240 1.36256 1.36248 58.28

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3 35 20 64 1.35670 1.35447 1.35559 35.31 1.36064 1.36024 1.36044 59.06
4 42 20 56 1.35189 1.35153 1.35171 28.85 1.35541 1.42801 1.39171 47.03
5 51 20 46 1.34134 1.34050 1.34092 10.87 1.44715 1.44434 1.44575 26.25
6 65 20 31 1.33895 1.33897 1.33896 7.60 1.46258 1.46261 1.46260 19.77

Figure 3: Equilateral Triangle Diagram for Acetone-Water-Toluene ternary system

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4.0 Discussion

The experiment conducted involved separation via liquid-liquid extraction. The method
is defined as the selective removal of one or more component from a liquid mixture by
using a second solvent, which can be completely or partially immiscible with the diluent.
For Experiments 1A and 1B, the water-rich phase is the raffinate while the toluene-rich
phase is the extract. For the Experiment 2, toluene was used as the solvent to remove the
solutes which is acetone from water, the diluent. This is because acetone is more
miscible in toluene compared to in water.
Figure 1 and Figure 2 were plotted based upon the results obtained in
Experiments 1A and 1B. By using the linear equation of a best fit line, y = mx + c, for
Experiment 1A, water is titrated in homogenous mixtures of acetone and toluene until a
cloud point is achieved. This cloud point, which represents one point on the binodal
curve, shows that equilibrium has been reached and may be validated after the mixture's
'cloudiness' no longer changes. As a result, negative gradient was obtained, indicating
the refractive index lowers as the weight percent of acetone increases in the light phase
which is the toluene-rich phase. For Experiment 1B, toluene is titrated in homogenous
mixtures of acetone and water. A positive gradient is obtained, indicating that the
refractive index increases as the weight percent of acetone increases in the heavy phase
which is the water-rich phase. The binodal curve was plotted based on the results
obtained, and it indicates points of any composition lying on it are in equilibrium.
In Experiment 2, the mixtures were agitated for a duration of 90 minutes then
settled in a separating funnel, as a result separated into the two phases: the heavy phase
and the light phase. The heavy phase is the raffinate phase rich in water, while the light
phase is the extract phase. The results obtained from Experiment 2 are used to construct
the tie lines connecting the binodal curve. These tie lines represent the condition at
which the extract phase and the raffinate phase exist in equilibrium. From the tie lines, it
is found that the extract phase always had a higher acetone composition than in the
raffinate phase. Thus, the liquid-liquid extraction is proven to be successful.

5.0 Error Analysis

There were perhaps some errors while we were conducting the experiments that might
have led to inaccuracies in the data obtained. First and foremost, the equipment used
such as measuring cylinder and burette have low sensitivities. Parallax errors might
have occurred while taking the readings (LearnPick, 2018). As a result, the weight
percent of the solutions prepared might not be accurately obtained. Second, errors might
have occurred while taking the readings during cloud-point titration: there is no standard
cloud point a reference therefore the cloudiness perceived might not be genuine. For
Experiment 2, while preparing the mixtures, some of the mixtures might not have been
covered immediately with paraffin film. As acetone and toluene are volatile, they might
have vaporized affecting the weight percent of the mixture. Besides, the mixtures might
not have separated well in the separating funnels into two distinctive layers with sharp

5
interface. Consequently, the refractive indices obtained might not be as accurate as
desired.

6.0 Conclusion
Liquid-liquid extraction involves the use of system consists of at least 3 components,
the solute, the solvent and the diluent, whereas the solvent and the diluent are two
wholly immiscible liquid. In the separation process, a second solvent which is partially
or completely immiscible with the feed, resulting in the solutes and the diluent separate
into two distinct phases. The equilateral triangle diagram is constructed as it
conveniently represents the data on the phase diagram. The main reason of constructing
the binodal curve and the tie lines is to find out the number of stages required in an
extraction tower to achieve a desired amount of solute in the extract feed. Other tie lines
can be obtained through interpolations on the Equilateral Triangle Diagram.
Based on Figure 1, it is noticed that as the weight percent of acetone increases, the
refractive index decreases in the toluene-rich phase. Meanwhile, the refractive index
increases as the weight percent of acetone increases in the water-rich phase, as can be
seen from Figure 2. From the data obtained in Experiment 2, it is found that acetone is
more soluble in toluene than in water as the toluene rich-phase always has a higher
acetone composition than the water-rich phase.

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7.0 Reference

Learnpick.in. 2018. How to Reduce Parallax Error. [online] Available at:

<https://www.learnpick.in/blog/how-to-reduce-parallax-
error#:~:text=Parallax%20error%20happens%20when%20the,that%20of%20the%
20device%20markings.> [Accessed 9 April 2022].
Sas, O., Domínguez, I., González, B. and Domínguez, Á., 2018. Liquid-liquid
extraction of phenolic compounds from water using ionic liquids: Literature review
and new experimental data using [C2mim]FSI. Journal of Environmental
Management, 228, pp.475-482

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8.0 Appendix
Experiment 1: Determination of Binodal/Solubility Curve
Physical properties of pure components of the ternary diagram are shown in the table
below.

Component Temperature (°C) Density (kgm-3) Viscosity (10-3 Pa)

Water 25 997.02 0.8903
Toluene 25 862.3 0.552
Acetone 25 784.4 0.304

Experiment 1A – Toluene Rich Phase

Sample calculation of the weight of pure components,
1m3 1000g
Weight g = Volume ml × Density (kgm−3 ) × ×
1000000ml 1kg

1 m3 1000 g
Weight of toluene = 97.0 ml × 862.3 kg. m−3 × × = ��. ���� �
1000000 ml 1 kg

1 m3 1000 g
Weight of water = 5.5 ml × 997.02 kg. m−3 × × = �. ���� �
1000000 ml 1 kg

1 m3 1000 g
Weight of acetone = 19.0 ml × 784.4 kg. m−3 × × = ��. ���� �
1000000 ml 1 kg

Sample calculation of the weight percentage of acetone and toluene,

Weight of acetone g
Weight percentage of acetone % = × 100
Total weight of pure component g
14.9036 g
Weight percentage of acetone % = × 100 = ��. ��%
83.6431 + 5.4836 + 14.9036 g

Weight of toluene (g)

Weight percentage of toluene (%) = × 100
Total weight of pure component (g)
83.6431 g
Weight percentage of toluene % = × 100 = ��. ��
83.6431 + 5.4836 + 14.9036 g

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Experiment 1B – Water Rich Phase
Sample calculation of the weight of pure components,
1m3 1000g
Weight g = Volume ml × Density (kgm−3 ) × ×
1000000ml 1kg

1 m3 1000 g
Weight of toluene = 18.8 ml × 862.3 kg. m−3 × × = ��. ���� �
1000000 ml 1 kg

1 m3 1000 g
Weight of water = 20.0 ml × 997.02 kg. m−3 × × = ��. ���� �
1000000 ml 1 kg

1 m3 1000 g
Weight of acetone = 83.0 ml × 784.4 kg. m−3 × × = ��. ���� �
1000000 ml 1 kg

Sample calculation of the weight percentage of acetone and toluene,

Weight of acetone g
Weight percentage of acetone % = × 100
Total weight of pure component g
65.1052 g
Weight percentage of acetone % = × 100 = ��. ��%
16.2112 + 19.9404 + 65.1052 g

Weight of toluene (g)

Weight percentage of toluene (%) = × 100
Total weight of pure component (g)
16.2112 g
Weight percentage of toluene % = × 100 = ��. ��%
16.2112 + 19.9404 + 65.10526 g

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Experiment 2: Determination of Equilibrium Solute Distribution (Tie Lines)

Sample calculation of the percentage weight of acetone for water rich phase and toluene
rich phase based on Experiment 1,

(a) Heavy Phase (Water rich phase)

Equation from Figure 1,

� = 0.0006� + 1.3344

where � = average refractive index;

� = weight percentage of acetone (%)

�−1.3344
�= 0.0006

When average refractive index, y = 1.36134,

1.36134−1.3344
�= 0.0006

� = ��. �%

(b) Light Phase (Toluene rich phase)

Equation from Figure 2,

� =− 0.0026� + 1.514

where � = average refractive index;

� = weight percentage of acetone (%)

�−1.514
� = −0.0026

When average refractive index,� = 1.36681,

1.36681−1.514
�= −0.0026

� = ��. ��%

10
Appendix A

11
Appendix B

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