Abstract

This experiment was conducted to study the distribution coefficient of K. The separating
funnel will be used for first experiment. The liquid/liquid extraction was used to carried out
for second experiment.The liquid/liquid experiment allow us to demonstrate the mass balance
and mass coefficient. In order to that, there are certain formulas that will be used. The
experiment These experiments required several data from the experiment like volume and
concentration of titration Sodium hydroxide, flow rate of aqueous and organic phase, etc. The
liquid/liquid extraction was maintained at constant flow rate for 20minutes. Then, the sample
can be taken from the experiment and proceed with titration with sodium hydroxide. After
calculated the desired based on the data, we were able to achieve the objectives of the
experiment conducted. This experiment was classified as successful.




















INTRODUCTION:
Liquid-liquid extraction have been applied in industry started from 1930s. This
equipment have been used in industrial operation. Some of the application of liquid-liquid
extraction are neutralization, purification of heat sensitive material and liquid-liquid
extraction for biotechnology. In this experiment, this equipment have been used in
experiment B which we need to demonstrate the mass balance that happen in the extraction
column. Besides that, we also need to measure the coefficient of mass transfer with the
aqueous phase as the continuous or batch medium. Liquid- liquid extraction is about
transferring solute to the solvent. For experiment A, we used titration process to determine
the distribution coefficient for the system organic solvent-Propionic Acid-Water also to show
its dependence on concentration. Sodium Hydroxide also have been used when this
experiment was performed. In addition, the function of liquid-liquid extraction is to separate
two immiscible the have been mixed that have unequal distribution of the component.



AIMS
The objective of experiment A is to determine the distribution coefficient for the
system organic solvent Propionic Acid Water and to show its dependence on concentration
.While experiment B is conducted for demonstrating how a mass balance is performed on the
extraction column and measuring the mass transfer coefficient with the aqueous phase as the
continuous medium.
Theory
Experiment A
The distribution coefficient, K also the defined as a ratio. The equation that have been used to
determine the distribution coefficient is:

K = Concentration of solute in the extract phase Y
Concentration of solute in the raffinate phase X

We assumed that the equilibrium exists between the two phase and at the low concentrations,
the distribution coefficient is dependence on the concentration. Then, Y=KX. The important
of K or distribution is to know the mass balance. After we know the mass balance, it is easier
for us to save energy. Save energy is important in industry because it includes overall cost of
production.
Next, Titration process have been used in experiment A. First of all, the solvent or in this
experiment we used deionized water or demineralization water (which ions inside the water
have been removed) have been mixed with Propionic acid or organic solvent which is
solution in this mixture. After that, the mixture have been allowed to be separate into two
parts which are, the raffinate phase and extract phase. Furthermore, the organic solvent with a
trace of propionic acid will be take the raffinate phase, while water and propionic acid will be
the extract phase.
Experiment B
There are all the equation involve to get the mass transfer coefficient. First of all, let:
V
w
= Water flow rate (l/ s)
V
o
= Organic solvent flow rate (l/s)
X = Propionic Acid concentration in the organic phase (kg/l)
Y = Propionic Acid concentration in the aqueous phase (kg/l)
1
= Top of column
2
= Bottom of column
Then, the mass balance:
V
o
(X
1
-X
2
) = Propionic Acid that have been extracted from the organic phase or raffinate
phase.
V
w
(Y
1
-0) = Propionic Acid that extracted from the aqueous phase which is extract phase.
Thus,
V
o
(X
1
-X
2
) = V
w
(Y
1
-0)

Next is the equation of extraction efficiency:
Mass transfer coefficient (based on the raffinate phase) =

Rate of acid transfer
(Volume of Packing)(mean driving force)


Then, log mean driving force =
2
1
ln
2 1
x
x
x x

Where,
x1 = Driving force at the top of the column = (X2 0)
x
2
= Driving force at the bottom of the column = (X
1
- X
1
*)
X
1
* is the concentration of organic phase that could be in equilibrium with concentration Y
1

that in the aqueous phase. In addition, the value of equilibrium can be known by using the
distribution coefficient that have been calculated from experiment 1.











APPARATUS
EXPERIMENT A
250ml conical stoppered flask
250ml measuring cylinder
250ml separating funnel
Pipette
MATERIALS
Sodium hydroxide solution(0.1M)
Phenolphthalein
Propionic acid

EXPERIMENT B
Liquid liquid extraction unit
Beakers
Measuring cylinders
Conical flasks
Retort stand
Burette
Separating funnel
MATERIALS
0.1M and 0.0025M NaOH
Phenolphthalein






PROCEDURE
Experiment A :
1) A mixture of 50 ml organic solvent and 50 ml deionised water was made up in a
conical flask.
2) 5 ml of propionic acid was added.
3) A stopper was placed into the flask and it had been shaken for 5 minutes.
4) Then the mixture was poured into the separating funnel and it had been left for 5
minutes and the aqueous layer had been removed.
5) Then the 100 ml of the layer had been taken and being titrated against 0.1M sodium
hydroxide solution using phenolphthalein as the indicator.
6) The experiment was repeated twice for initial additions for propionic acid were 3 ml
and 1ml.
Experiment B :
1) 100 ml of propionic acid was added into 10 litres of the organic phase.The mixture
had been mixed well to ensure an even concentration.Then the organic phase feed
tank was filled with the mixture,
2) The level control to the bottom of column was switched.
3) The water feed tank was filled with 15 L of clean deionised water then the water feed
pump started while the column was filled with water at high flow rate.
4) The flowrate was reduced to 0.21 L/min as the water is above the top of packing.
5) The metering pump was started and the flowrate was set to 0.21 L/min.
6) The extraction column was ran fo 15 minutes until steady condition was achieved.
7) Then 15 ml samples from feed,raffinate and extract stream were taken.
8) Each 10 ml sample were titrated against 0.1 M sodium hydroxide solution using
phenolphthalein as the indicator.






DISCUSSION
EXPERIMENT A
For the first experiment,the distribution coefficient for the system organic solvent-
propionic acid water was calculated by using the formula K=Y/X,in which Y represents the
concentration (M) of propionic acid in aqueous layer while X represents the concentration of
propionic acid in organic layer.Aqueous layer is the extract of the mixture and it is the
product that contains the removed material whereas the organic layer is the raffinate,the
liquid streams that remains after solutes from original liquid is removed through contact with
immiscible liquid.Water acts as the solvent whilst the organic solvent-propionic acid is
solution to be separated into extract and raffinate phase.Water comes in contact with the
solution and the propionic acid is separated from the organic solvent.10 ml of the lower
aqueous layer from the experiment was obtained and was titrated with 0.1M of NaOH
solution to neutralised the acid.Hence,the concentration of the propionic acid from the sample
can be calculated.The concentration of the propionic acid (solute) is vital for the
determination of the distribution coefficient (K).
From the experiment,the concentration of solute(propionic acid)is greater in aqueous
layer (Y) than that of in the organic layer(X).Thus,propionic acid has great miscibility with
water than in the organic solvent.For example,the concentration of propionic acid in the
aqueous layer for 5ml propionic acid added is 1.68 M while for the organic layer the
concentration of propionic acid is less that is only 1.32 M.
Distribution coefficient (K) is defined as the ratio of the amount of solutes dissolved
in two immiscible liquids at equilibrium.In this experiment,water and organic solvent were
used as the immiscible liquids.From the results,the distribution coefficient (K) of the
propionic acid increased when less amount of propionic acid was added into the
solution.Thus,distribution coefficient is dependent on the acid concentration.At
equilibrium,Y=KX is proven.
EXPERIMENT B
In experiment B,the mass transfer coefficient of propionic acid at different transfer
rate and driving force was determined.The experiment was conducted at constant flow rate of
aqueous phase and organic phase, 0.21 L/min.Samples were taken from the feed,raffinate and
extract valves of the liquid-liquid extraction unit respectively and were titrated against 0.1M
and 0.025M NaOH solution to be neutralised.Hence,the concentration of propionic acid in
each samples can be determined.
Results shows that the concentration of propionic acid in the raffinate phase is greater
than that of in the extract phase.These results are different as we compared with the results of
experiment A.In experiment A,the concentration of propionic acid is larger in the extract
phase than in the raffinate phase.Hence,we can say that liquid-liquid extraction unit has
different effect on mass balance of solutes.
The mass balance of propionic acid was determined by calculating the rate of
propionic acid transfer in both raffinate and extract phase.We compare the rate of propionic
acid transfer by using the formula:
For 0.1 M NaOH :
min / 0294 . 0
min
0294 . 0
) 0 ( ) (
1 2 1
mol
mol
y V X X v
w o

For 0.025 M NaOH :

min / 0247 . 0
min
0247 . 0
) 0 ( ) (
1 2 1 0
mol
mol
y V X X V
w

Hence,mass balance of propionic acid in each phase is achieved.
However,different rate of acid transfer gives different mass transfer coefficient value.For
example,when the rate of acid transfer is 0.0294 mol/min,the mass transfer coefficient is
0.5191 kg/min while when the rate of acid transfer is 0.0247 mol/min,the mass transfer
coefficient is 0.56624 kg/min.These are due to certain conditions such driving force in top
and bottom columns and different concentration of acid added.


Conclusion
Based on our experiment and the result. We can conclude the experiment was succeed as we were
able to achieve the objectives of the experiment. For experiment A, the concentration (M) of
propionic acid in aqueous layer, Y proportional to the concentration of propionic acid in
organic layer, X. When less amount of propionic acid was added, distribution coefficient (K)
of the propionic acid increased. Thus, prove the equation Y=KX. For experiment B, we did
achieve the aims of the experiment despite the result were the same as experimental value.
This was probably because the liquid/liquid extraction giv the different effect on mass
balance of solutes
RECOMMENDATION
For this experiment , there are some precaution steps that I want to recommend .
Firstly , I suggest we should wear a lab coat with long hand before enter the lab and while
conducting the experiment. Then, the important part is we should wear a safety cap when
enter the pilot plant and while conducting the experiment to prevent any head injury
.Then during taking the reading for volume NaOH used for titration,we must place our
eyes perpendicular to the scale reading to get accurate reading.Lastly while conducting
the experiment, we should wear a gloves and goggles to protect our hand and eyes from
any hazardous and toxic substances .Besides that, do not wear contact lens while
conducting the experiment because it can easily be effect by the toxic, thus can give
harmful to our eye .

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