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UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA


HEAT & MASS TRANSFER LABORATORY
(CHE504)
NAME: STUDENT NO :
MUHAMAD IBNU HAKIM BIN SHUHAINI 2017632072
MOHAMAD NORAFIQ BIN ZULKEPLI 2017632138
NORHAYATI BINTI AB RAHMAN 2017632114
NURUL NAJIHAH BINTI JAAFAR 2017632056
NURLINA SYAHIIRAH BINTI MD TAHIR 2017632214
GROUP : EH2204I
EXPERIMENT : LIQUID – LIQUID EXTRACTION (L7)
(GROUP REPORT)
DATE PERFORMED : 3rd MAY 2018
SEMESTER :4
PROGRAMME / CODE : CHEMICAL ENGINEERING / EH220
SUBMIT TO : MADAM SYAFIZA BINTI ABD HASHIB

No. Title Allocated Marks (%) Marks


1 Abstract/Summary 5
2 Introduction 5
3 Aims 5
4 Theory 5
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100

Remarks:

Checked by: Rechecked by:

--------------------------- ---------------------------Date:
Date:
TABLE OF CONTENT

1.0 ABSTRACT ................................................................................................................... 2

2.0 INTRODUCTION......................................................................................................... 3

3.0 OBJECTIVES ............................................................................................................... 4

4.0 THEORY ....................................................................................................................... 5

5.0 MATERIALS & APPARATUS ................................................................................... 8

6.0 METHODOLOGY ....................................................................................................... 9

7.0 RESULTS .................................................................................................................... 12

8.0 CALCULATIONS ...................................................................................................... 15

9.0 DISCUSSION .............................................................................................................. 20

10.0 CONCLUSION ........................................................................................................... 23

11.0 RECOMMENDATIONS............................................................................................ 24

12.0 REFERENCES ............................................................................................................ 25

13.0 APPENDICES ............................................................................................................. 26

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 1


1.0 ABSTRACT

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 2


2.0 INTRODUCTION

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.

K is the distribution coefficient which is the ratio at equilibrium of the solute


concentration in extract and raffinate phases. The distribution coefficient gives the measure of
the affinity of the solute for the two phases. Liquid – liquid Extraction Unit UOP5 is the
equipment used for the experiment to run the separation process of system organic solvent (B)
– propionic acid (A) – water (C) in order to determine the K value of the system and its
dependence on the concentration of propionic acid in extract and raffinate phases. The water
solvent and the feed solution (propionic acid and organic solvent) is mixed and allowed to
separate intro extract phase and raffinate phase. The extract phase is water (C) – propionic acid
(A) whereas the raffinate is organic solvent (B) with a trace of propionic acid (A).

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 3


3.0 OBJECTIVES

The objectives for this experiment are:

1) To determine the suitable methodology for the experiment,


2) To determine the distribution coefficient, K for the system organic solvent – propionic acid
– water,
3) To show the dependence of the K value on the concentration of the solute at raffinate and
extract phase,
4) To determine the mass transfer coefficient of propionic acid based on the K value obtained,
5) To determine how mass balance is conducted on the extraction column.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 4


4.0 THEORY

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

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 5


will be removed from the top when the solvent is denser than carrier liquid and the solvent fed
into the top of the column. Therefore, counter current frequently high solubility of two liquid
phases in each other

Figure 2 - Counter Current Extraction Unit

Furthermore, the selection of solvent in liquid-liquid extraction is important in order to


achieve maximum transfer of the solute from the carrier into the solvent. There are a few
characteristics of ideal solvent that need to be choose to ensure that the extraction will
completely miscible with the carrier and have a high affinity for solute molecules. The solvent
that has a high solubility of solute and low solubility of carrier liquid is the ideal solvent that
must be chosen in liquid- liquid extraction process. Besides, the solvent which nonreactive with
the other chemical involved in the extraction and has high boiling temperature are suitable for
liquid-liquid extraction process. In dilute solution at equilibrium, the concentration of solute in
two phases are called the distribution coefficient, K.

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;

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 6


Transfer rate of propionic acid to the extract phase (Extract from aqueous phase):

Transfer rate of propionic acid to the raffinate phase (Extract from organic phase):

Log Mean Driving Force:

X* = The concentration of Propionic Acid in the organic phase which would be in equilibrium

with the concentration of propionic acid in the aqueous phase.

Mass Transfer Coefficient:

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 7


5.0 MATERIALS & APPARATUS

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 8


6.0 METHODOLOGY

6.1 General Start Up – LLE Equipment


1) All the valves on the equipment is closed including the drain valves. The longest
and middle electrodes at top of the extraction column and the shortest and middle
electrodes at bottom of column are ensure to be approximately 5mm apart.
2) Tank L2 is filled up with tap water.
3) The equipment is then connected to the electrical supply.
4) The electrode switch is set to top position (Switch S2). Main Switch S1 is operated.
Switch S3, S4 and S5 is ensure to be OFF and switch S1 is illuminated. Solenoid
valve C3 is opened by ensuring the light in on. The electrode switch is set to
bottom position. Then, the solenoid valve C3 is once again checked to ensure the
valve still open.
5) Valve V3 is then open and the water pump is switch on using switch S3. The water
pump is allowed to prime (water discharge at V3), then the vent valve V3 is closed.
6) The control valve C1 is opened. The water flow is checked on flowmeter F1. The
water delivered to injector at base of extraction column is checked.
7) The column is allowed to start filling with water at a slow rate. The solenoid valve
C3 is opened until water covers the short electrode, then the valve is closed. The
drain valve V11 at the base of the extraction column is opened and water is drain
until the tip of the short electrode is exposed and then valve C3 is opened once
again.
8) The drain valve V11 in base of column is then closed. The control valve C1 is the
opened and adjusted to give full scale reading on flowmeter F1. The solenoid valve
C3 is then closed again when the water level reaches the short electrodes. Then the
column is gradually filled. The electrode switch is leaved in the down position. The
solenoid valve C3 is still closed. Then, wait until the column completely full with
water. The water flows is ensure to flow from the top of the column to the
polythene sorage tank L1.
9) Electrodes Switch S2 is then set to top position. The solenoid valve C3 is ensure to
remains closed. The flowmeter control valve C1 is closed. The drain valve V11 at
the base of the column is opened and water is allowed to drain until the water level
falls below the long electrode. The solenoid valve C3 is checked and ensure open.
The water drained into tank L3 until level in columns equals level in tank L3.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 9


10) The pipework and the column are checked in case of leaking.

6.2 Experiment A* – Determination of the Distribution Coefficient, K


1) 50mL of trichloroethylene is mixed with 50mL de-mineralized water in a conical
flask.
2) 5mL of propionic acid is added into the conical flask by using a dropper.
3) A stopper is placed on the flask mouth and the conical flask is then shook for 5
minutes. Then, the mixture is poured into a separating funnel and left for 5 minutes.
4) 10mL of the bottom layer (Raffinate) is taken as the sample and 3 drops of
phenolphthalein is added. The sample is then titrated using 0.1 M Sodium
hydroxide solution until light pink solution is formed.
5) The remaining bottom layer is removed until the upper layer (Extract) can be taken.
6) 10mL of the extract sample is taken and 3 drops of phenolphthalein is added into
the sample. The sample is then titrated using 0.1 M Sodium hydroxide solution
until light pink solution is formed.
*Experiment A is unable to be conduct due to lack in materials at the respective date of
the experiment. The data for experiment A is obtained from previous group experiment
(Appendix B).

6.3 Experiment B – Determine the Mass Transfer Coefficient

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 10


8) Then, 15mL of each sample is taken and 3 drops of phenolphthalein is added into
each sample.
9) All the sample is then titrated with 0.1 M Sodium hydroxide solution until light
pink solution is formed.
10) Step 8 is repeated and the sample is titrated using 0.025M Sodium hydroxide
solution until light pink solution is formed.

6.4 General Shut Down – LLE Equipment


1) The water pump is switch off.
2) All liquid in the feed tank and product tank is drained.
3) All the piping is flush with clean water.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 11


7.0 RESULTS

7.1 Experiment A – Determination of Distribution Coefficient, K


Table 1 - Distribution Coefficient, K for the System

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).

Graph of Volume Propionic Acid Added into System vs


Distribution Coefficient, K
1.94
1.92
Distribution Coefficient, K

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 12


7.2 Experiment B – Determination of Mass Transfer Coefficient
Table 2 - Volume Flow rate of Organic Phase and Aqueous Phase

Flow rate (L/min)


Aqueous Phase, VAP 0.2
Organic Phase, VOP 0.2

Table 3 - Volume of Sodium Hydroxide Used For Samples Titration

Volume of Sodium Hydroxide (mL)


Concentration 0.025 M 0.1 M
Feed 253.8 81.5
Raffinate 4 2.2
Extract 52 15.9

Table 4 - Concentration of Propionic Acid in the 100mL of the Respective Samples

Concentration of Propionic Acid (M)


Concentration of Sodium Hydroxide 0.025 M 0.1 M
Feed, X1 0.0635 0.0815
Raffinate, X2 0.0010 0.0022
Extract, Y1 0.0130 0.0159

Table 5 - Mass Flow Rate of Propionic Acid in the Sample Phases and Percentage of
Propionic Acid Missing From the System

Mass Flow rate (g/min)


Concentration of Sodium Hydroxide 0.025 M 0.1 M
Feed, X1 0.9408 1.2075
Raffinate, X2,E 0.0148 0.0326
Extract, Y1 0.1926 0.2356
Percentage Missing (%) 77.95 77.79

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 13


Table 6 - Calculated Data for Mass Transfer Coefficient, kc

Concentration of Sodium Hydroxide, NaOH


0.025 0.1000
solution (M)
Transfer Rate of Propionic Acid, ̇ @ ̇
0.0026 0.0032
(mol/min)
Concentration of Propionic Acid in Raffinate,
0.0505 0.0655
X2,T (M)
Percentage Error of Concentration of Propionic
98.02 96.64
Acid in Raffinate, X2 (%)
K Value 1.9272 1.8415 1.9272 1.8415
X* 0.0067 0.0071 0.0083 0.0086
Log Mean Driving Force (mol/min) 0.0536 0.0534 0.0693 0.0691
Mass Transfer Area (m2) 0.0079
Mass Transfer Coefficient, kc (x 10-3 m/s) 6.1402 6.1632 5.8451 5.8620

Graph of Distribution Coefficient, K values versus Mass Transfer


Coefficient, kc
Mass Transfer Coefficient, kc x 10^-3

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

Figure 5 - Graph of Distribution Coefficient, K values against Mass Transfer


Coefficient, kc for 0.025 M and 0.1 M Sodium Hydroxide Solution
The graph shows that the mass transfer coefficient decreases with increase in
distribution coefficient and concentration of Sodium hydroxide, NaOH used to neutralize the
propionic acid.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 14


8.0 CALCULATIONS

EXPERIMENT A* – DETERMINATION OF DISTRIBUTION COEFFICIENT


Sample Calculation for Concentration of Propionic Acid

Sample Calculation for Distribution Coefficient, K

* 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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 15


EXPERIMENT B – DETERMINATION OF MASS TRANSFER COEFFICIENTS
Sample Calculation for Concentration of Propionic Acid in Feed

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.

Sample Calculation of Mass Flow rate of Propionic Acid in Feed

̇ ̇

̇ ( ) ( )( )

̇ 1.2075 g/min
̇
̇

(74.08 g/mol) (Information)

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 16


Sample Calculation for Transfer Rate of Propionic Acid at Extract, ̇ (Extracted From
Aqueous Phase)

̇ ( )( )

The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.

Sample Calculation of Concentration of Propionic Acid in Raffinate Phase using Transfer


Rate of Propionic Acid value

̇ ̇

( )( )

The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 17


Sample Calculation of Error of Concentration of Propionic Acid in Raffinate Phase

The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.

Sample Calculation for X* from Distribution Coefficient, K

The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.

Sample Calculation for Log Mean Driving Force

( )

The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 18


Sample Calculation for Mass Transfer Area, A

Sample Calculation for Mass Transfer Coefficient

( )

The calculation is then repeated for the K-value = 1.9272. The calculation is then repeated for
0.025M of Sodium Hydroxide, NaOH solution.

Sample Calculation for Percentage of Missing Propionic Acid in the System

( )

The calculation is then repeated for 0.025M of Sodium Hydroxide, NaOH solution.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 19


9.0 DISCUSSION

Liquid-liquid extraction (LLE) is a chemical process of extraction solute from a mixture by


using a solvent. In this experiment, we are extracting propionic acid from trichloroethylene-
propionic acid mixture by using water as solvent. After experiment has been done, sample from
feed, raffinate, and extract were taken to determine the concentration of propionic acid present.
This experiment was carried out to determine the distribution coefficient and mass transfer
coefficient of LLE. Distribution coefficient, K also known as partition coefficient is the
concentration ratio of between extract and raffinate. Meanwhile, mass transfer coefficient is
defined as rate constant of diffusion between 2 compounds.

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%

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 20


for 0.025 M. From the data, the experimental value is too low which resulting in the
assumption of that the propionic acid in raffinate phase is definitely lower than it supposed to
be. The source of error could also due to the feed of the system itself. Based on the volume of
sodium hydroxide needed to neutralize the acid, feed is having very high concentration of
propionic acid. Since, K value depends on the concentration of propionic acid in the feed, very
high concentration will resulting in very low K value. Thus, the distribution of the propionic
acid towards extract and raffinate is very low. Besides, due to this fact, the propionic acid is
distributed more towards extract and only small amount left for the raffinate.

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 21


Mass transfer coefficient is the diffusion rate constant that related with mass transfer
rate, area and concentration change. In order to calculate the mass transfer coefficient, the data
of log mean driving force is needed. The log mean driving force for K value of 1.9272 for
0.1M is 0.0693 and 0.025M is 0.0536, while the value for K value of 1.8415 is 0.0691 and
0.0534 for K value of 0.1M and 0.025M respectively. Therefore, we can find the mass transfer
coefficient by using formula stated in the calculation part. Mass transfer coefficient for K value
of 1.9272 is 6.1402x10-3 m/min and 5.8451x10-3 m/min for concentration of 0.025M and 0.1M
respectively, while 6.1632x10-3 m/min (0.025M) and 5.8620x10-3 m/min (0.1M) for K value of
1.8415. Based on Figure 5, the mass transfer coefficient decreases with the increase in
distribution coefficient, K value and concentration of sodium hydroxide, NaOH solution used
for the sample to reached end point.

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 22


10.0 CONCLUSION

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 23


11.0 RECOMMENDATIONS

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.

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 24


12.0 REFERENCES

Lab Manual. (March, 2018). Retrieved from I-Learn.

Geankoplis, C. J. (1993). Transport Processes and Unit Operations (Third Edition ed.).
Minnesota: Prentice Hall International Inc.

Information, N. C. (n.d.). Propionic Acid. Retrieved 7 June, 2018, from PubChem:


https://pubchem.ncbi.nlm.nih.gov/compound/propionic_acid#section=Top

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

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 25


13.0 APPENDICES

Appendix A

Figure 7 - Data Results Obtained For Experiment B

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 26


Appendix B

Figure 8 - Previous Group Data Results for Experiment A that have been referred for
this experiment

LAB REPORT ON LIQUID – LIQUID EXTRACTION (L7) 27

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