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TABLE OF CONTENT
2.0 INTRODUCTION......................................................................................................... 3
11.0 RECOMMENDATIONS............................................................................................ 24
Liquid-liquid extraction is one of the separation technology used in industries. This process is
quite different with distillation because it focuses on relative solubility of the species rather
than volatility. Usually, extraction is more preferable than distillation for separation application
that is not cost efficient and applicable for distillation. This experiment was carried out to
determine the distribution coefficient and mass transfer coefficient of LLE. The sample
collected from extraction equipment, namely raffinate, extract and feed were titrated with
sodium hydroxide with different concentration. An indicator, phenolphthalein were added into
the sample in order to detect alkaline ion. The sample is titrated until the solution turns light
pink. The amount of 0.025M sodium hydroxide needed to turn the colourless feed, extract and
raffinate solution to light pink were 253.8 mL, 52 mL and 4 mL respectively. While for 0.1M
sodium hydroxide, the samples need 81.5 mL, 15.9 mL and 2.2 mL in the same order as
mentioned previously. The mass transfer coefficients in 0.025M NaOH are 6.1402x10-3 m/min
and 6.1632x10-3 m/min for K value 1.9272 and 1.8415 respectively. Meanwhile, for 0.1M
NaOH, the mass transfer coefficients are 5.8451x10-3 m/min and 5.8620x10-3 m/min for K
value 1.9272 and 1.8415 respectively. As the concentration of sodium hydroxide, NaOH
solution and the distribution coefficient, K values increases, the mass transfer coefficient of
propionic acid will decreases. The experiment is considered successful since all the objectives
are successfully achieved.
Liquid – liquid Extraction is a process that separates components based on the chemical
differences rather than differences in physical properties. The basic principle for this process is
a mixture is contacted with another insoluble liquid solvent that is immiscible with the original
but the miscible with the specific solute in the original solution. The transfer is based on the
preferential solubility of solute in feed with the solvent. Solvent rich solution containing the
desired extracted solute is the extract, whereas the residual feed solution containing little solute
is the raffinate. This two phase are formed after the addition of the solvent due to the
differences in densities.
Liquid – liquid extraction is a process that separates the components mixture based on their
relative solubility in two immiscible or miscible liquid. Liquid – liquid extraction involves
solute and solvent that are mixing together in order to separates the products. Firstly, liquid
stream which function as a carrier that contain the solute (component to be recovered) is fed
into an extractor of liquid – liquid extraction unit and the solute will be directly contacts with a
solvent. In order to allow the mixture to form dispersion which one liquid dispersed as droplet,
the two liquid needs to be immiscible and only slightly miscible (Geankoplis, Transport
Processes and Unit Operations, 1993).
In liquid-liquid extraction units, mass transfer occurs when the surrounding liquid react
with the droplets. The different densities of the liquid subsequently separate the two liquids and
the accumulation of the droplets from the above or below continuous phase occurs depending
on the liquids relative densities. The droplet dispersion at the top and bottom of the extraction
column.
Figure 1 - Extraction Unit of Two Inlet Streams (The Liquid Barrier Containing Solute
Molecules and Solvent) And Two Outlet Streams (Raffinate And Solute-Rich Extract)
Usually liquid-liquid extraction being carried out in continuous staged units involved
whether co-current or counter-current flow. In terms of multiple stages extraction, counter
current mixing most preferred rather than co-current because counter- current is amenable to
multi-stages per unit while co-current only limited only for one theoretical stage (Joerg Koch,
2015). Besides, in extraction process the arrangement of the counter-current extractor depends
on the density solvent and solute carrier which means that solvent less-dense than the carrier
liquid will be fed in the bottom of the column while the solute carried to the top of extractor
and the carrier liquid will remove from the bottom unit. Otherwise, the carrier steam carrier
The transfer rate of the propionic acid from organic solvent to water solvent will be
dependent on the area of the interface to be formed by droplets and films, the situation being
analogous to that existing in packed distillation column. The mass balance theory for the
system organic solvent (B) – propionic acid (A) – water (C) as follows;
Transfer rate of propionic acid to the raffinate phase (Extract from organic phase):
X* = The concentration of Propionic Acid in the organic phase which would be in equilibrium
5.1 Materials
1) 0.1 M Sodium Hydroxide, NaOH solution
2) 0.025 M Sodium Hydroxide, NaOH solution
3) Phenolphthalein
4) Trichloroethylene
5) Propionic Acid
6) De-mineralized water
5.2 Apparatus
1) Burette
2) 250mL measuring cylinder
3) 250mL Conical Flask
4) 250mL Beaker
5) 250mL separator funnel
6) Stopper
7) Liquid – liquid Extraction Unit UOP5
(a) (b)
Figure 3 - Liquid - Liquid Extraction Unit UOP5 Used in The Experiment (a) Front
View, (b) Side View.
1) 100mL of propionic acid is added to 10L of the organic phase before the mixture is
mixed.
2) The electrode switch S2 is set to bottom position.
3) The water feed tank is filled with 15mL clean de-mineralized water, then the water
pump is started to fill the column with water at a high flow rate.
4) The flow rate of the water is reduced to 0.20 L/min as the water reached the top of
the column.
5) The metering is then started and the flow rate is set at 200 L/min.
6) The experiment is run for 20 minutes until steady conditions are achieved.
7) Sample from the feed, raffinate and extract stream are taken 100mL each and the
liquid – liquid extraction unit is shut down.
Propionic Aqueous Layer (Y), Extract Organic Layer (X), Raffinate Distribution
Acid Added Titre* Concentration Titre* Concentration Coefficient,
(mL) (mL) (M) (mL) (M) K
3 53 1.7667 27.5 0.9167 1.9272
5 94.1 1.8820 51.1 1.0220 1.8415
* The data is obtained from previous group experiment since experiment B needs the K value
obtained from experiment A for determination of mass transfer coefficient of propionic acid at
the respective samples in Experiment B (Appendix B shows the result obtained for experiment
A from the refer group).
1.9
1.88
1.86
1.84
1.82
1.8
1.78
3 5
Volume of Propionic Acid Added into System, mL
Figure 4 - Graph of Propionic Acid Added into the System against Volume against
Distribution Coefficient, K
The graph shows that the greater the volume of propionic acid added into the system,
the smaller the value of distribution coefficient, K.
Table 5 - Mass Flow Rate of Propionic Acid in the Sample Phases and Percentage of
Propionic Acid Missing From the System
6.2
6.1
6
(m/s)
5.9
0.025M
5.8 0.1M
5.7
5.6
1.8415 1.9272
Distribution Coefficient, K values
* The sample calculation is for system added with 5mL Propionic Acid. The calculation is then
repeated for the system added with 3mL Propionic Acid. The K value for 0.025M of Sodium
Hydroxide solution is assumed to be the same as 0.1M due to lack of data for the experiment.
The calculation is then repeated for Extract and Raffinate phase. The calculation is also
repeated for the respective phases at 0.025M of Sodium Hydroxide, NaOH solution.
̇ ̇
̇ ( ) ( )( )
̇ 1.2075 g/min
̇
̇
The calculation is then repeated for Extract and Raffinate phase. The calculation is also
repeated for the respective phases at 0.025M of Sodium Hydroxide, NaOH solution.
̇ ( )( )
The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.
̇ ̇
( )( )
The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.
The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.
The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.
( )
The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.
( )
The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.
( )
The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.
This experiment has been done by titrating sodium hydroxide into the samples collected
from liquid – liquid extraction equipment. The samples which are collected from feed, extract
and raffinate were titrated by using two different concentration of sodium hydroxide solution
which is 0.1 M and 0.025 M. Before the titration, phenolphthalein was added into the sample in
order to detect the alkaline ions from sodium hydroxide solution. As sodium hydroxide
solution added into the conical flask containing the sample, it will change the sample colour
from colourless to pink colour. The volume of 0.025M sodium hydroxide solution needed to
turn the solution from colourless to pink for feed, extract and raffinate were 253.8 mL, 52 mL
and 4 mL respectively. While for 0.1M sodium hydroxide solution take 81.5 mL, 15.9 mL and
2.2 mL for feed, extract and raffinate sample respectively. From the data collected on the
titration, the concentration of propionic acid is determined at each phase.
For this experiment, K-value cannot be determined due to lack of chemical resources at
the date of the experiment. Therefore, we took the data for Experiment A from previous group
that have done the experiment with the same variable, constant and methodology as the
reference data for our experiment as in Appendix B. Based on Figure 4, the graph shows that
the greater the volume of propionic acid added into the system, the smaller the distribution
coefficient, K. Thus, high concentration of propionic acid in the system will reduce the
distribution coefficient, K. Based on Table 1, the distribution of the propionic acid move
towards extract higher than towards raffinate.
For the mass balance part, by assuming that the propionic concentration in extract and
feed follows the theoretical value, the concentration of propionic acid in raffinate, X2 is used to
determine the percentage error for the experiment. The results show that X2,Theory and
X2,Experimental is vary with very high percentage error of about 97% for 0.1 M NaOH and 98%
This high percentage of error could also be explained with the percentage of propionic
acid missing as the process of extraction going on is also very high of about 78% for both
concentration of Sodium Hydroxide solution. The reason could also due to the probability of
the system having not reached the equilibrium state but the sample for raffinate and extract
have been taken. Figure 6 shows the three phases after they reached their end point with
Raffinate phase required the least volume of sodium hydroxide to reached end point and Feed
the largest.
Figure 6 - The titrates of the three phases which from the left side is Extract Phase,
Raffinate Phase and Feed Phase respectively.
During the experiment, there were several errors that been made and may influence the
results obtained. One of the error can be seen from the large different in volume of sodium
hydroxide titrated in 0.025M for the feed sample. The data collected was 253.8 mL which so
large compare to result in 0.1M sodium hydroxide which is 81.5 mL. From the result, we can
assume that the huge different in data is based on the common error made by student mistake in
order to titrated the solution. Then, the other error that been made throughout the experiment
was unstandardized colour of pink solution. In order to get the precise data, the colour of pink
solution should be standardized throughout all the titration process as same colour. In this
experiment, we have made an error when all the titrated solution have slightly different colour
and it affect the distribution coefficient and mass transfer coefficient value.
The distribution coefficient, K values for 3ml and 5mL indicates that increase in the
concentration of propionic acid, decreasing the distribution coefficient, K values with both
volumes indicates that the concentration of propionic acid in extract is larger than in the
raffinate. Percentage error of the concentration of propionic acid in the raffinate phase, by
assuming that the feed and extract phase follow theoretical mass balance approximately 97%
for 0.1M NaOH solution and 98% for 0.025M NOH solution. The percentage of propionic acid
missing for both NaOH concentrations is approximately 78%. It is believed the large
percentage errors are contributed by the large percentage of propionic acid missing within the
process. Based on the result above, mass transfer coefficients in 0.025M NaOH are 6.1402x10-3
m/min and 6.1632x10-3 m/min for K value 1.9272 and 1.8415 respectively. Meanwhile, for
0.1M NaOH, the mass transfer coefficients are 5.8451x10-3 m/min and 5.8620x10-3 m/min for
K value 1.9272 and 1.8415 respectively. It can be concluded that when the concentration of
sodium hydroxide, NaOH solution and the distribution coefficient, K values increase, the mass
transfer coefficient of propionic acid will decrease. From the experiment, it can be concluded
that the experiment is successful as all the objectives of the experiment were determined.
Although the experiment was proven a success, there are several recommendations that
students can apply to increase the quality of experiment conducted. Students should ensure that
their eyes are perpendicular to the meniscus while using the measuring cylinder to avoid
parallax error. The students should also ensure the titration is done carefully and slowly since
the end point of the titration process can comes abruptly. Besides that, students should also
wear proper PPE (personal protective equipment) such as gloves while conducting this
experiment to avoid the chemical used from made contact with the skins. Students also need to
properly familiarize themselves with the separation equipment and the apparatus used for the
experiment to ensure the experiment is done in a correct manner so that accurate data is
obtained. Last but not least, students should conduct the experiment for at least twice to ensure
accuracy of the data obtained.
Geankoplis, C. J. (1993). Transport Processes and Unit Operations (Third Edition ed.).
Minnesota: Prentice Hall International Inc.
Joerg Koch, G. S. (November, 2015). Design Principles For Liquid - Liquid Extraction.
Retrieved 7 June, 2018, from AiCHE:
https://www.aiche.org/resources/publications/cep/2015/november/design-principles-
liquid-liquid-extraction
Wikipedia. (n.d.). Mass Transfer Coefficient. Retrieved 7 June, 2018, from Wikipedia:
https://en.wikipedia.org/wiki/Mass_transfer_coefficient
Appendix A
Figure 8 - Previous Group Data Results for Experiment A that have been referred for
this experiment