Faculty of Petroleum &

Renewable Energy
Engineering

LAB REPORT SKKK 3731

SEPARATION PROCESSES LABORATORY I
2016/2017 – 02
EXPERIMENT 5
TITLE : LIQUID LIQUID EXTRACTION
LAB INSTRUCTOR Dr Muhammad Tahir
SECTION : 05
GROUP NO. : 6
GROUP MEMBERS No. Name NRIC
1. THRISHNAA BALASUPUR MANIAM 950709026160
2. LELAVATHY SAMIKAN 950111146328
MAZILAMANI
3. NOR MUHAMAD BIN MOHD 950513105801
SIDDIKI
4 MOHD ASIK BIN SHABICK 951220145935
5 MUHAMAD IQBAL BIN NOOR AZIZI 950125146329

DATE OF : 9.04.2017
EXPERIMENT
DATE OF : 16.04.2017
SUBMISSION
GRADING SECTION

Criteria Score Comment Total Mark

Cover page, Abstract / Table of Content
Introduction/Theory/
Literature Review
Experimental procedure/Methodology
Raw data and analysis
Results & Discussion
Conclusion and Recommendations
Job Safety Analysis/References
Tables of Content Pages
Abstract 1
Table of Contents 2
1.0 INTRODUCTION
1.1 Experimental Background 3
1.2 Objective 3
1.3 Scope of experiment 4
2.0 THEORY 5
3.0 METHODOLODY
3.1 Equipment and Materials 9
3.2 Experimental Procedure 10
4.0 RESULTS AND DISCUSSION 11
5.0 CONCLUSION 25
6.0 RECOMMENDATIONS 25

References 26
Appendices 27
1.0 INTRODUCTION

1.1 Experimental Background

Absorption is the incorporation of a substance in one state into another different state for example
liquids being absorbed by solid or gases being absorbed by a liquid. In this experiment, it is the absorption
of a gas into a liquid. The absorption of a gas into a liquid is one of the fundamental processes of industrial
chemistry. It makes it possible to separate on more components of a gaseous mixture and to produce a
liquid containing desired quantity of a gas.
There are several equipments for absorption process and the most common used absorption towers are
plate (tray) tower and also packed tower. This experiment is to investigate the flooding point characteristic
of packed tower. Packed tower is used for continuous countercurrent contacting of gas and liquid in
absorption. As the current process usage is learning more toward packed towers and especially structured
packing, it will concentrate on vertical packed tower design. In countercurrent flow, the tower must be
designed to prevent flooding which occurs when the upward flow of the gas is of sufficient velocity to
prevent the liquid flow from coming down the tower. If the gas velocity is too high, it will lead to a point
known as flooding point whereby the liquid filled the entire tower and the operation became difficult to
carry out. High pressure will damage the packings in the tower.
The driving force for the mass transfer in absorption is the concentration difference of the solute
between the gaseous and liquid phases. The driving force can be interpreted as the difference between the
partial pressure of the soluble gas in the gas mixture and the vapor pressure of the solute gas in the liquid
film in contact with the gas. However, the higher the gas velocity, the greater the resistance that will be
encountered by the down-flowing liquid and the higher the pressure drop, ∆P across the packings.
 1.2 Objective of experiment
The objectives of this experiment are:
i. To determine the flooding point and its velocity through the observation and data of the experiment.
ii. To investigate the effects of gas and water flow rate on the flooding point in absorption tower.
iii. To analysis the relation and effects between the changes of gas and water flow rate towards pressure
drop, ∆P.

1.3 Scope of experiment

The experiment was done to study the flooding point and the flooding velocity in the Raschig ring
absorption packed tower. The parameters such as gas and water flow rate has to be manipulated to observed
the flooding point of the absorption tower. The changes of water and gas flow rate indirectly affected the
pressure drop.
2.0 THEORY

Absorption

Absorption (also known as scrubbing) is a process which separates a solute or several solutes from a gas
phase by contacting the gas with a liquid phase. This process involves molecular and turbulent diffusion or
mass transfer of solute A through a stagnant, non-diffusing gas B into a stagnant liquid C. The fundamental
physical principles apply in the absorption process are the solubility of the absorbed gas and the rate of mass
transfer. One or more of the components dissolve in the liquid and thus be removed from gas mixture. There are
two types of absorption processes, physical absorption and chemical absorption. For physical absorption, the
gaseous component forms a physical solution with the liquid or the solvent. For chemical absorption, the solute
reacts with the liquid chemically.

There are two possible methods of contacting the gas and liquid which are counter-current operation and
co-current operation. Gas absorption is usually carried out in vertical counter current columns. The solvent is
fed at the top of the absorber whereas the gas mixture enters from the bottom. The absorbed substance is
washed out by the solvent and leaves the absorber at the bottom as a liquid solution. The absorption column
maybe a packed column, plate column, spray column, venturi scrubbers, bubble column, falling films, wet
scrubbers or stirred tanks. The absorption process is usually applied on gas purification, product recovery,
production of solutions of gases for various purposes and post-combustion systems.

Packed Absorption Column

Absorption columns or towers are commonly used for continuous countercurrent contacting of gas and
liquid in absorption. A soluble vapor is absorbed from its mixture with an inert gas by means of a liquid in
which the solute gas is more or less soluble. The packed column consists of a cylindrical column containing a
gas inlet and distributing space at the bottom, a packing or filling in the tower. There are a liquid inlet and
distributor at the top of the column. The gas and liquid are flow out from the top and bottom of the column
respectively. The gas enters the distributing space below the packed section and rises upward through the
openings or interstices in the packing and contacts the descending liquid flowing through the same openings.
The column packing is to ensure a large area of intimate contact between the liquid and the gas.

Column Packing

There is various types of tower packing have been developed and some are used quite often. The
principal requirements of a packing are that it should provide a large surface area for better contact between gas
and liquid phase; it should have an open structure to lower the resistance of gas flow; it should promote uniform
liquid distribution on the packing surface and it should promote uniform vapour gas flow across the column
cross-section. The packing can be divided into two broad classes; packings with regular geometry (stacked
packings or structured packings) and random packings.

Stacked packings have sizes of 75mm or so and larger are also used. The packing is stacked vertically,
with open channels running uninterruptedly through the bed. It is usually used for high gas rates, where low
pressure drop is essential, for example, in cooling towers. However the gas-liquid contact in stacked packings is
poorer than the others two.

The term structured packing refers to packing elements made up from wire mesh or perforated metal
sheets. The material is folded and arranged with a regular geometry, to give a high surface area with a high void
fraction. They are available in metal, plastics and stoneware. The advantage of structured packings is their low
HETP and low pressure drop compared to random packings. They are used for difficult separation and have
higher efficiency than random packings.

Common types of random packing are Raschig ring, Pall ring, Berl saddle, Intalox saddle, Metal Hypac
and Super Intalox as shown in Figure 2.1. Ceramic Raschig rings are one of the oldest types of random packing
and are still in general used. It reduces the pressure drop and maintain economy and efficiency compared to
others. Pall rings are essentially Raschig rings in which openings have been made by folding strips of the
surface into the ring. This increases the free area and improves the liquid distribution characteristic. Berl
saddles were developed to give improved liquid distribution compared to Raschig rings. The latest generation
packings are the Intalox saddles, which are a combination of the Berl saddle and the Pall ring; their shape
makes them easier to manufacture than Berl saddles. The Metal Tri-Pack is a Pall ring in spherical shape. The
latter two are slightly more efficient than the Pall rings. The Hypac and Super Intalox can be considered
improved types of Pall rings and Intalox saddles respectively. The packings of the column may be constructed
from clay, porcelain, metal or plastic. The bed of packing rests on a support plate should be designed to have
high void spaces of 65-95% so that it can permit relatively large volumes of liquid to pass countercurrent to the
gas flow through the openings with relatively low pressure drop.
Figure 2.1. Types of packing: (a) Raschig rings; (b) Pall ringsl; (c) Berl saddle ceramic; (d) Intalox saddle
ceramic; (e) Metal Hypac; (f) Ceramic Super Intalox.
Pressure Drop and Flooding in Packed Column

In packed column the gas and liquid rates are limited by the tendency of the column to flood. Flooding
velocity is the upper limit to the rate of gas flow in a given packed column with a given type and size of packing
and with a definite flow of liquid. The column cannot operate above this gas velocity. At low gas velocities the
liquid flows downwards through the packing, essentially uninfluenced by the upward gas flow. As the gas flow
rate is increased at low gas velocities, the pressure drop is proportional to the flow rate to the 1.8 power.

∆P  Gas flow rate 1.8

As either liquid or gas velocity is increased, the liquid holdup or accumulation in the packing increases,
the free area for gas flow decreases, and the pressure drop through the column increases. A point is finally
reached when the gas bubbles violently through the liquid, the pressure drop rises extremely sharply with the
slightest increase in gas velocity, and much liquid is carried off mechanically by the gas leaving the top of the
packing. This point is called the flooding point or loading point and is determined by both gas and liquid rates.

In an actual, operating tower, the gas velocity is well below flooding. The optimum economic gas
velocity is about one-half or more of the flooding velocity. It depends upon a balance of economic factors
including equipment cost, pressure drop and processing variables. Pressure drop in the packing is an important
consideration in design of a tower.

In the report, the effect of variation of air flow rate and water flow on the flooding and pressure drop
will be discussed.
 4.0 RESULTS

4.1 Experimental result

The experimental data below shows the changing of heavy phase flow rate with constant light phase flow rate.
For each data of extract composition was recorded for every 5 minutes until the valid of data is obtained. The
data of raffinate composition was recorded too after obtaining the constant data of extract composition.

Table 4.1: Result of extract composition, raffinate composition and time

Extract Composition (g/L) Time (min)

Heavy phase flow rate : 0.0423 5

10 L/min 0.0592 10

0.1015 15

Light phase flow rate : 0.0761 20

15 L/min 0.0508 25

0.0423 30

0.0423 35

0.0423 40

Raffinate Composition Time (min)

(g/L)

1.6074 45

Extract Composition (g/L) Time (min)

Heavy phase flow rate : 0.0592 5

15 L/min 0.0508 10

0.0508 15

Light phase flow rate : 0.0508 20

15 L/min

Raffinate Composition Time (min)

(g/L)
 1.4890 25

Extract Composition (g/L) Time (min)

Heavy phase flow rate : 0.0338 5

20 L/min 0.0338 10

0.0.338 15

Light phase flow rate :

15 L/min Raffinate Composition Time (min)

(g/L)

1.4213 20

4.2 Sample of calculation

Concentration of Iodine In Raffinate or Extract (g/L)

2S2O32- (aq) + I2 (aq) 2I- (aq) + S4O62- (aq)

Molecular Weight for I2 = 253.8 g / mol

Concentration Na2S2O3 = 0.01 M

Volume of raffinate sample = 30 mL

0.01 mol S 2 O32 253.8 g I 2 1 mol I 2 1

[I 2 ]   Volume Na 2 S 2 O3 mL   2

L mol I 2 2 mol S 2 O 3 30 mL

= Volume Na2S2O3 mL x 0.0423 g/L

First set of data for extract:

Volume of Na2S2O3 used = 2.4 mL

0.01 mol S 2 O32  253.8 g I 2 1 mol I 2 1

[I 2 ]   2.4 mL Na 2 S 2 O3   2

L mol I 2 2 mol S 2 O 3 30 mL

= 0.10152 g/L
First set of data for raffinate:

Volume of Na2S2O3 used = 38 mL

0.01 mol S 2 O32  253.8 g I 2 1 mol I 2 1

[I 2 ]   38 mL Na 2 S 2 O3   2

L mol I 2 2 mol S 2 O 3 30 mL

= 1.6074 g/L
5.0 DISCUSSION

Figure 4.1: Graph of extract composition versus time taken

i) State which component is the heavy phase, light phase, solvent, and solute.

In this experiment, water is the heavy phase, which flew as the bottom layer. Hexane, on the other hand,
was the light phase that flew as the upper layer.

Iodine was the solute which was soluble in hexane, the solvent.

ii) State the dispersed phase and thecontinuous phase in this experiment.

In this experiment, hexane is the dispersed phase while water was the continuous phase.

In liquid-liquid extraction, there are two phases of liquids that are insoluble in each other, which then
form two immiscible layers during liquid-liquid extraction, called dispersed phase and continuous phase.
Hexane is classified as dispersed phase as it forms many small bubbles that dispersed in another phase
continuously. On the other hand, water was classified as static phase as it looked static during the experiment.

The rate of separation of emulsion will be faster if the size of the bubbles of dispersed phase is bigger,
and the difference in densities of the two layers is bigger. For stable emulsion, dispersed phase with bubbles
bigger than 1mm in diameter will settle down faster. The tendency of bubbles to group together is higher than
their surface tension.

iii) What is the meaning ofequilibrium contact?

 It refers to the equilibrium achieved among the components (iodine, hexane and water) at maximum
point of extraction. At the starting of the extraction, the concentration of iodine in hexane layer is higher than
that in the water layer. However, as the extraction process was carried on, the concentration of iodine in the
hexane decreased, while that in water layer increased. After a certain period, the equilibrium contact was
achieved between the three components, and the extraction process stopped. At this stage, the separation of
iodine from the hexane layer had reached the maximum point, and the composition raffinate layer and extract
were constant.

iv) Discuss the effect of flow rate towards the extraction efficiency.

From the experiment, it was observed that the efficiency of extraction is directly proportional to the flow
rate of the dispersed phase and continuous phase. The higher the flow rate of the two layers, the higher is the
efficiency of extraction. When the flow rate of raffinate layer is small, the time needed for the raffinate layer to
achieve constant composition was longer.

This happens as the increase in flow rate increases the rate of contact between the two immiscible
layers. Countercurrent flow of the two layers also increased the total contacting area and time of contact
between the two layers. When flow rate increased, the collision of molecules in the liquids increased, therefore
more iodine was extracted from the hexane layer to the water layer, until the contact equilibrium was achieved.

v) State others steps and measures to be taken toincrease the performance of this extraction process.

 Make sure all the apparatus used are cleaned before starting the experiment.
 In order to avoid parallax error, the eyes of the observer have to be at the same level as the scale
when using measuring cylinder to take the sample. It is recommended that all the readings are
taken by the same person.
 Make sure same amount of starch is used in each time of the titration.
 Titration has to be done drop by drop as the colour of the starch is not obvious. A white paper
has to put under the conical flask during the titration for a better vision.
 Repeat the taking of samples until the raffinate composition is constant.

vi) Describe the importance of liquid-liquid extraction processes in chemical engineering.

 To extract precious metal.

 The generation of two immiscible water phases, which then can be used to extract protein which
denature when exposed to organic solvents.
 Remove unwanted solute in the dispersed phase.
 Used to separate aromatics from aliphatic compounds.
 Recovery of antibiotics from fermentation broths.
 Recovery and separation of vitamins.
  Production of alkaloids from natural products.

The errors that might occurred in the experiment.

 The pump might not function effectively, affecting the water flow.
 There might be some residue left in the measuring cylinder and conical flask after each cleaning,
affecting the result of the titration.
 The addition of starch affect the concentration of the water sample in titration.
 Difficulties in determining the end point of the titration, especially when determining the
raffinate composition due to the disappearance of colour.
 There might be parallax error when taking the reading of water sample in measuring cylinder, or
during titration.
 Sodium thiosulphate solution may be contaminated which and affected the accuracy in titration.
6.0 CONCLUSION

Based on the results the time take for the stable iodine content in the sample with heavy phase flow rate
of 10L/min, 15L/min, and 20L/min was 40 min, 20 min and 15 min respectively. When the flow rate of
the heavy phase increases, steady state can be achieved faster. In this experiment, the time taken for the
system to achieve steady state was short (fast process) when the heavy phase flow rate increases. In
conclusion, the performance of the extraction process increases with the flowrate.
6.0 RECOMMENDATIONS

PROBLEM SOLUTION

Data collected not accurate. Repeat experiment more than one time and
take the mean value.

Time to finish the experiment Read and analyze the steps and concept of
insufficient. the experiment before the lab session to
minimize time and ensure the time allocate
for the experiment is enough.

Incorrect reading/data based on Checked the machine thoroughly to make

the instrument. sure that there are no damage or leakage,
so that, the data that will be obtained are
correct and no accident may happened.
REFERENCES

1. Geankoplis, C. J.(1995), “Transport Processes & Unit Operations”, 3rd Edition, Prentice.
2. Jose V. Herrez and R. Belda. (2006). “Refractive Indices, Densities and Excess Molar
Volumes of Monoalcohols + Water”. Springer Science + Business Media, Inc.
3. J. D. Seader and Ernest J. Henley (1998). Separation Process Principles, Wiley, U.S.A.
4. Mc Cabe et.al., (1985)’Unit Operation of Chemical Engineering’, 4th Edition, Mc Graw-Hall.
5. Packed Column Distillation, Retrived from http://cuo2.kkft.bme.hu/packed.pdf
6. Richard and Patricia (2004). ‘Principles of chemical separation with environmental
applications’ Terry Cambridge University press, Cambridge.

9.0 APPENDICES

Concentration of Iodine In Raffinate or Extract (g/L)

2S2O32- (aq) + I2 (aq) 2I- (aq) + S4O62- (aq)

Molecular Weight for I2 = 253.8 g / mol

Concentration Na2S2O3 = 0.01 M

Volume of raffinate sample = 30 mL

0.01 mol S 2 O32 253.8 g I 2 1 mol I 2 1

[I 2 ]   Volume Na 2 S 2 O3 mL   2

L mol I 2 2 mol S 2 O 3 30 mL

= Volume Na2S2O3 mL x 0.0423 g/L

Initial data for raffinate:

Volume of Na2S2O3 used = 55.8 mL

= 2.36034 g/L