Fall 2016 Lab Manual - CHEG455 (Sec 51 & 52) PDF

STUDENT
LABORATORY MANUAL
CHEG455 (Sec 51 & 52)
CHEMICAL ENGINEERING LABII

(Heat Transfer and Mass Transfer)
THE PETROLEUM INSTITUTE

Fall 2016
PREFACE
This laboratory manual is prepared for CHEG455 lab course (Chemical Engineering laboratory II
course) of the chemical engineering program. It is divided in two sections namely Heat Transfer
(SectionI) and Mass Transfer (SectionII). It is designed to serve as a laboratory handout for
students. It covers all aspects of the course and describes briefly about conducting the experiments
in the lab, report writing and oral presentation.
A. Syed Ali
Fall 2016
CHEG455: CHEMICAL ENGINEERING LAB II
II
TABLE OF CONTENTS
S. No.
Page No.
Preface.ii
Table of Contents....iii
Section I: Heat Transfer

1. Shell and Tube Heat Exchanger
..5
2. Plate Heat Exchanger
.......13
3. Linear Heat Conduction
............................21
4. Radial Heat Transfer
.30
Section II: Mass Transfer

5. Wetted Wall Column
6. Absorption in Packed Column
..38
44
7. Immiscible Liquid Liquid Extraction
..52
8. Distillation of Cyclohexanen Heptane
..56
CHEG455: CHEMICAL ENGINEERING LAB II
III
Section I
Heat Transfer
EXPERIMENT
ONE
SHELL & TUBE HEAT EXCHANGER
INTRODUCTION AND EQUIPMENT DESCRIPTION

The shell and tube heat exchanger is commonly used in the refining, food and chemical process industries. This
type of heat exchanger consists of a number of tubes in parallel enclosed in a cylindrical shell. Heat is
transferred between one fluid flowing through the tubes and another fluid flowing through the cylindrical shell
around the tubes. Baffles inside the shell increase the velocity of the fluid and hence the rates of heat transfer.
Figure 1 : Process schematic of GUNT WL 110 series heat Exchanger with service Unit
A computer compatible tubular heat exchanger; (GUNT WL 110.03 series heat Exchanger) with service
Unit will be used. The service unit acts as a base unit onto which different heat exchangers can be installed and
CHEG455 CHEMICAL ENGINEERING LAB II
studied. It provides the pump, the cold water circulation system and a temperature controlled hot water
circulation system. Also, it provides flow control valves and thermocouple temperature sensors to monitor the
heat exchanger process. In normal operation the hot fluid from the hot water circulator enters the header at
one end of the shell and passes through the bundle of stainless steel tubes. The cold fluid from the cold water
supply passes through the cylindrical shell. This arrangement minimizes heat loss from the exchanger without
the need for additional insulation and allows the construction of the exchanger to be viewed. The outer
annulus, caps and baffles are constructed from clear acrylic to allow visualization of the heat exchanger
construction and minimize thermal losses. These provide a liquid seal, accommodate differential expansion
between the metal and plastic parts and allow the inner metal tubes to be removed for cleaning. Four
thermocouple temperature sensors measure the inlet and exit temperatures of the cold and hot streams. This
miniature exchanger has one shell and seven tubes with two transverse baffles in the shell.
PART # A
A1. OBJECTIVES
To investigate the effect of changes in hot and cold fluid flowrates on the temperature efficiencies and overall
heat transfer coefficient.
A2. APPROACH
By performing the experiment at different combinations of hot and cold fluid flowrates, measuring the fluid
temperatures and calculating the corresponding overall heat transfer coefficient.
A3. THEORY/ BACKGROUND

Any temperature difference across the metal tube wall will result in the transfer of heat between the two fluid
streams. The hot water flowing through the inner tube bundle will be cooled and the cold water flowing
through the outer shell will be heated.
A3.1. Temperature Efficiency

(a) Countercurrent Operation
In countercurrent configuration of the heat exchanger hot and cold fluid streams flow in opposite directions
across the heat transfer surface (the two fluid streams enter the heat exchanger at opposite ends). The hot fluid
passes through the seven tubes in parallel, the cold fluid passes across the tubes three times, directed by the
baffles inside the shell.
Figure 2: Flow Pattern and Temperature Profile in Countercurrent Shell and Tube Heat Exchanger
Reduction in hot fluid temperature T = T1 - T2
(C)
Increase in cold fluid temperature T
(C)
hot
cold
= T4 - T3
Heat power emitted from hot fluid Q = qm . (Cp) (T1 - T2)
(W)
Heat power absorbed by cold fluid, Qa = qmc.Cpc (T4 T3)
(W)
Heat power lost or gained, Qf = Qe Qa
(W)
Overall efficiency,
Qa
x100
Qe
(%)
A useful measure of the heat exchanger performance is the temperature efficiency of each fluid stream. The
temperature change in each fluid stream is compared with the maximum temperature difference between the
two fluid streams giving a comparison with an exchange of infinite size.
Temperature efficiency of a stream is given by,
Temperature change in stream

Maximum temperature difference between stream
Temperature efficiency for hot fluid h =
T1 T2
.100
T1 T3
Temperature efficiency for cold fluid c =

Mean Temperature Efficiency m =
T4 T3
.100
T1 T3
h + c
2
(%)
(%)
(%)
(%)
(b) Cocurrent Operation
In cocurrent configuration of the heat exchanger, hot and cold fluid streams flow in the same direction across
the heat transfer surface (the two fluid streams enter the heat exchanger at the same end). The hot fluid passes
through the seven tubes in parallel, the cold fluid passes across the tubes three times, directed by the baffles
inside the shell.
Figure 3: Flow Pattern and Temperature Profile of Cocurrent Shell and Tube Heat Exchanger
Reduction in hot fluid temperature, Thot =
T2 T1
(C)
Increase in cold fluid temperature, Tcold =
T4 T3
(C)
Heat power emitted from hot fluid, Qe= qmh. (Cp)h (T2 T1)
(W)
Temperature efficiency for hot fluid, h =
T2 T1
.100
T2 T3
(%)
Temperature efficiency for cold fluid, c =
T4 T3
.100
T2 T3
(%)
Mean Temperature Efficiency, m =
h + c
2
(%)
A3.2. Overall Heat Transfer Coefficient

Because the temperature difference between the hot and cold fluid streams varies along the length of the heat
exchanger it is necessary to derive an average temperature difference (driving force) from which heat transfer
calculations can be performed. This average temperature difference is called the logarithmic mean temperature
difference (LMTD), t .
lm
LMTD, t lm =
t 1 t 2
t
ln 1
t 2
(t t )
1
Where, t =
(T2 T3)
(C)
and t =
(T1 T4)
(C)
LMTD, t lm =
(T2 T3 ) (T1 T4 )
(T T3 )
ln 2
(T1 T4 )
Note : In this exercise, LMTD equation is same for both countercurrent and cocurrent operation.
Heat transmission area in the exchanger must be calculated using the arithmetic mean diameter of inner tubes.
do + di
2
Arithmetic mean diameter, d
Heat transmission length, L
= n. l
Where, n = number of tubes
=7
l, heat transmission length of each tube

L
(m)
(m)
= 0.144
(m)
=1.008
2
= . d .L
Heat transmission area, A
(m )
(d can be used since r2/r1<1.5 otherwise the logarithmic mean radius d must be used)
m
lm
Overall heat transfer coefficient, U =
Qe
A.t lm
(W/m
o C)
A4. RESULT & DATA ANALYSIS

o
For each set of readings, plot the temperature profile of the heat exchanger. Comment on basic features and
differences between cocurrent and countercurrent flow configuration.
Comment on the effect of flow configuration (cocurrent/countercurrent) on driving force (Thot and Tcold) of
the heat exchanger.
Plot and comment on the effect of variables (hot and cold water flowrates).on efficiencies (cold water, hot
water, mean) and overall heat transfer coefficient.
Comment on the effect of flow configuration (cocurrent/countercurrent) on mean efficiencies and overall heat
transfer coefficient.
Calculate and comment on cumulative influence of the experimental errors on your calculated parameters (i.e.
temperature efficiencies, LMTD, heat transfer coefficient). Due to the limitation of the thermocouples and
other associated instrumentation, temperature measurement will incur some error, which propagates further,
when used for calculations.
PART # B
B1. OBJECTIVES
To investigate the effect of driving force with cocurrent and countercurrent flow
B2. APPROACH
As described in part A
B3. THEORY/ BACKGROUND

As described in part A
B5. RESULT & DATA ANALYSIS

o
Comment on the variation of efficiencies (cold water, hot water, mean) and overall heat transfer coefficient
with studied variable (hot water temperature).
Comment on the effect of flow configuration (cocurrent/countercurrent) on mean efficiencies and overall
Estimate the influence of the experimental errors on your calculated values for log mean temperature
difference and overall heat transfer coefficient. Due to the limitation of the thermocouples and other
associated instrumentation, temperature measurement will incur some error, which propagates further,
In previous exercises if you have calculated overall heat transfer coefficient of another type of heat
exchanger (i. e. plate heat exchanger, jacketed vessel heat exchanger and shell and tube heat exchanger),
compare the performances of these heat exchanger and comment on the differences.
Operating the Heat Exchanger Unit

o
Observe all safety precautions
Set the main power switch to position 1 from 0
Check the water level in hot water tank
Open cold water feed at the cold water mains
Open the regulator for cold water (V2)
Open the regulator for hot water (V1)
Start the pump (P)
Set the desired hot water set point on the TIC controller
Set the desired cold water flow rate Vc; using regulator valve V2
Set the desired hot water flow rate Vh; using regulator valve V1
Switch on the heater
Make settings for the measured value file, start automatic measured value recording
Observe the measured values. Wait until a steady state is reached
Save screen shots for the time response of measured value and the current temperature in a file.
When the experiment is complete, first turn off the heater
Then stop the pump
Close the regulator valves V1 & V2
Close the cold water feed at the mains
Set the main switch to 0
10
Note: Refer Appendix A for nomenclature and detailed specifications of the Shell & Tube Heat Exchanger
Appendix A: Nomenclature and Technical Specification of Shell & Tube Heat Exchanger
Nomenclature
Name
ID/OD of tube
Arithmetic mean diameter of tube
Symbol
d/ d
i
Heat transmission length

Heat transfer area
L
A
SI unit
m
m
m
2
m
kJ/kgK
Specific heat capacity hot fluid
Cp
Specific heat capacity cold fluid
Cp
Hot fluid inlet /outlet temperature
T1/T2
Cold fluid inlet/outlet temperature
T3/T4
Decrease in hot fluid temperature
Increase in cold fluid temperature
hot
cold
hot
cold
kJ/kgK
Driving force, hot fluid inlet
Driving force, hot fluid outlet
Logarithmic mean temperature difference
Volume flowrate (hot fluid)
qv
hot
m /s
Volume flowrate (cold fluid)
qv
cold
m /s
Density of hot fluid
kg/m
Density of cold fluid
Mass flowrate hot fluid
qm
kg/m
kg/s
Mass flowrate cold fluid
qm
C
C
C
3
3
hot
cold
hot
cold
Heat power absorbed by cold fluid
Heat power lost (or gained)
Overall efficiency
Temperature efficiency hot fluid
Temperature efficiency cold fluid
Mean temperature efficiency
lm
Heat power emitted from hot fluid
Overall heat transfer coefficient
e
a
f
hot
cold
mean
3
3
kg/s
W
W
W
%
%
%
%
2
W/m C
11
Technical Specification:
WL 110.03 Shell & Tube Heat Exchanger
12
EXPERIMENT
TWO
PLATE HEAT EXCHANGER
INTRODUCTION AND EQUIPMENT DESCRIPTION
The plate heat exchanger is extremely versatile and commonly used in pharmaceutical, food and chemical
processing industries where different combinations of plates and gaskets can be arranged to suit a
particular application. The GUNT WL 110.02 plate heat exchanger is a miniature scale version of a typical
industrial plate heat exchanger.
Figure 1 : Process schematic of GUNT WL 110 series heat Exchanger with service Unit
A computer compatible tubular heat exchanger; (GUNT WL 110.03 series heat Exchanger) with service
Unit will be used. The service unit acts as a base unit onto which different heat exchangers can be installed
and studied. It provides the pump, the cold water circulation system and a temperature controlled hot
water circulation system. Also, it provides flow control valves and thermocouple temperature sensors to
13
monitor the heat exchanger process. The exchanger unit consists of six
plates with sealing gaskets held
together in a frame between a fixed end plate and moving end plate. Two nuts/bolts passing through the end
plates compress the plates and gaskets together. Hot and cold fluids flow between channels on alternate sides
of the plates. The plate heat exchanger supplied is configured for multi-pass operation with passes in series.
Hot and cold fluid flows may be configured for either cocurrent or countercurrent operation. Each end plate
incorporates tappings for the hot and cold fluids to enter/leave the exchanger and sensors in each of the
tappings allow the temperatures of the fluids to be measured. The direction of flow (countercurrent or
cocurrent) can be controlled by altering the tubing configuration. The four thermocouple temperature sensors
measure the inlet outlet temperatures of cold and hot water fluids. The fittings are color coded red for hot
water and blue for cold water to aid identification. In normal countercurrent operation, T1 and T2 refer to the
inlet and outlet temperature of hot water, while T3 and T4 refer to the inlet and outlet temperatures of the cold
water respectively.
Figure 2: Plate Heat Exchanger GUNT WL 110.02
A1. OBJECTIVES
PART # A
To investigate the effect of changes in hot and cold fluid flowrate on the temperature efficiencies and overall
A2. APPROACH
By measuring the fluid temperatures at different combinations of hot and cold fluid flowrate then calculating
the corresponding overall heat transfer coefficient
A3. THEORY/ BACKGROUND

The hot and cold fluids flow between channels on alternate sides of the plates. Each stream passes three times
in series across the plates. Any temperature difference across the metal plates will result in the transfer of heat
14
between the two fluid streams. As the streams pass through the pack of plates the hot water will be cooled and
the cold water will be heated.
A.3.1. Temperature Efficiency

(a) Countercurrent Operation
In a countercurrent configuration of plate heat exchanger, hot and cold fluids enter at opposite ends. However,
the flows are not truly countercurrent throughout the exchanger because the flow on either side of the plates is
not always in the opposite direction as shown below.
Figure 3: Flow Pattern and Temperature Profiles in Countercurrent Plate Heat Exchanger
Reduction in hot fluid temperature Thot =
T1 - T2
(C)
Increase in cold fluid temperature Tcold =
T4 - T3
(C)
Heat power emitted from hot fluid Qe =
qmh. (Cp)h (T1 - T2)
(W)
Heat power absorbed by cold fluid Qa =
qmc. (Cp)c (T4 - T3)
(W)
A useful measure of the heat exchanger performance is the temperature efficiency of each fluid stream. The
temperature change in each fluid stream is compared with the maximum temperature difference between the
two fluid streams giving a comparison with an exchanger of infinite size.
Temperature efficiency for hot fluid h =
T1 T2
.100
T1 T 3
(%)
15
Temperature efficiency for cold fluid, c =

Mean temperature efficiency, m =
T4 T3
.100
T1 T 3
(%)
m +m
(%)
(b) Cocurrent Operation

When the heat exchanger is connected for cocurrent operation the hot and cold fluids enter the exchanger
at the same end. However, the flows are not truly cocurrent throughout the exchanger because the flow
on either side of the plates is not always in the same direction as shown below.
Figure 4: Flow Pattern and Temperature Profile in a Cocurrent Plate Heat Exchanger
Reduction in hot fluid temperature, Thot=
T2 T1
(C)
Increase in cold fluid temperature, Tcold =
T4 T3
(C)
Heat power emitted from hot fluid, Qe=
qmh.(Cp)h (T2 T1)
(W)
Heat power absorbed by cold fluid, Qa =
qmc.(Cp)c (T4 - T3)
(W)
Temperature efficiency for hot fluid, h =
T2 T1
.100
T2 T 3
Temperature efficiency for cold fluid, h =

T4 T3
.100
T2 T 3
(%)
(%)
16
Mean temperature efficiency, m =
m +m
(%)
A.3.2. Overall Heat Transfer Coefficient

Heat power emitted from hot fluid;
Countercurrent operation
Qe = qmh.(Cp)h (T1 - T3)
(W)
Cocurrent operation;
Qe = qmh.(Cp)h (T3 T1)
(W)
Because the temperature difference between the hot and cold fluid streams varies throughout the heat
exchanger it is necessary to derive an average temperature difference (driving force) from which heat transfer
calculations can be performed. This average temperature difference is called the logarithmic mean temperature
difference (LMTD) tlm.
LMTD t lm =
t1 t 2
ln t1
t 2
(t1 t2)
Where,
t1 = (T2 T3)
(C)
t2 = (T1 T4)
(C)
LMTD t lm =
t1 t 2
ln t1
t 2
(C)
Note: In this example the equation for LMTD is the same for both countercurrent and cocurrent operation because the temperature
measurement points are fixed on the exchanger. Two different equations will result if the temperature points are related to fluid inlets and
outlets.
Overall heat transfer coefficient, U =
Qe
A.F .t lm
(W/m2K)
A4. RESULT & DATA ANALYSIS

o
For each set of readings, plot the temperature profile of the heat exchanger. Comment on basic features
and differences between cocurrent and countercurrent flow configuration.
Comment on the effect of flow configuration (cocurrent/countercurrent) on driving force (Thot and
Tcold) of the heat exchanger.
Plot and comment on the effect of variables (hot and cold water flowrates).on efficiencies (cold water, hot
water, mean) and overall heat transfer coefficient.
17
Calculate and comment on cumulative influence of the experimental errors on your calculated parameters
(i.e. temperature efficiencies, LMTD, heat transfer coefficient). Due to the limitation of the thermocouples
and other associated instrumentation, temperature measurement will incur some error, which propagates
further, when used for calculations.
PART # B
B1. OBJECTIVES
To investigate the effect of driving force with cocurrent and countercurrent flow
B2. APPROACH
As described in Part A.
B3. THEORY/ BACKGROUND

As described in Part A.
Operating the Heat Exchanger Unit

o
o
o
o
o
o
o
o
o
o
o
o
o
o
o
o
o
o
o
Observe all safety precautions

Set the main power switch to position 1 from 0
Check the water level in hot water tank
Open cold water feed at the cold water mains
Open the regulator for cold water (V2)
Open the regulator for hot water (V1)
Start the pump (P)
Set the desired hot water set point on the TIC controller
Set the desired cold water flow rate Vc; using regulator valve V2
Set the desired hot water flow rate Vh; using regulator valve V1
Switch on the heater
Make settings for the measured value file, start automatic measured value recording
Observe the measured values. Wait until a steady state is reached
Save screen shots for the time response of measured value and the current temperature in a file.
When the experiment is complete, first turn off the heater
Then stop the pump
Close the regulator valves V1 & V2
Close the cold water feed at the mains
Set the main switch to 0
B4. RESULT & DATA ANALYSIS

o
Comment on the variation of efficiencies (cold water, hot water, mean) and overall heat transfer coefficient
with studied variable (hot water temperature).
18
Estimate the influence of the experimental errors on your calculated values for log mean temperature
difference and overall heat transfer coefficient. Due to the limitation of the thermocouples and other
associated instrumentation, temperature measurement will incur some error, which propagates further,
In previous exercises if you have calculated overall heat transfer coefficient of another type of heat
exchanger (i. e. tubular heat exchanger, jacketed vessel heat exchanger and shell and tube heat exchanger),
compare the performances of these heat exchanger and comment on the differences.
19
Appendix C: Nomenclature and Technical Specification of Plate Heat Exchanger
Nomenclature
Name
Number of active plates
Projected heat transfer area of each plate
Symbol
N
a
SI Unit
Dimensionless
Total heat transmission area
Specific heat capacity hot /cold fluid

Hot fluid inlet/outlet temperature
Cp / Cp
hot
cold
T1/T2
m
kJ/kgK
Cold fluid inlet/outlet temperature
T3/T4
Decrease in hot fluid temperature
Increase in cold fluid temperature
Driving force, hot fluid inlet
Driving force, hot fluid outlet
Logarithmic mean temperature difference
Volume flowrate (hot fluid)
qv
m /s
Volume flowrate (cold fluid)
qv
m /s
Density of hot/cold fluid

Mass flowrate cold fluid
/
hot
cold
qm
kg/m
kg/s
Heat power emitted from hot fluid
Heat power absorbed by cold fluid
Heat power lost (or gained)
Overall efficiency
Temperature efficiency hot/cold fluid
Mean temperature efficiency
/
hot
cold
LMTD correction factor
Dimensionless
Overall heat transfer coefficient
W/m C
2
2
hot
cold
C
C
2
mean
C
3
hot
cold
cold
e
a
f
mean
W
W
%
2
Technical Specification
Number of active plates, N:
Dimension Length X Width X Height
400 X 230 X 85 mm
Weight
3 Kg
Plate Material
Stainless steel
Heat Transfer area
0.048 m2
20
EXPERIMENT
THREE
LINEAR HEAT CONDUCTION
Introduction
This experiment is designed to demonstrate the fundamental of heat transfer by linear conduction through
a metallic material (solid conduit). The heat transfer will be exhibited by monitoring of temperature at
various locations in a solid sample (specimen of steel, brass and aluminum) using thermocouples placed at
designated locations. The schematic if the temperature, flow, voltage and current in the equipment is given
below.
(a)
(b)
Figure 1: Temperature distribution in linear heat conduction heat transfer with (part b) and without (part a)
intermediate sample/specimen
21
Figure 2 : Linear and radial heat conduction apparatus
The WL 372 Heat Conduction Unit is a tabletop (figure 2)unit with two experimental arrangements,
linear conduction (1) and radial conduction (2). The storage vessels serve as storage locations for the
inserts (3).The control and display unit (4) is placed near the study unit. The two units are connected
together via two cables, a data cable (5) and a power cable (6). A laboratory cooling water feed and
return system and mains power complete the experimental setup
Objectives:
The main objective of this experiment is as follows:
A. To measure the temperature distribution for steady state conduction of energy through a uniform
plane wall and demonstrate the effect of a change in heat flow.
B. To understand the use of the Fourier Rate Equation in determining rate of heat flow through solid
materials for one dimensional, steady flow of heat.
Linear Conduction
The setup for linear conduction (1) comprises three elements:
- fixed part with heater (1.1)
- moveable part with cooler (1.4)
- Various inserts
22
By opening the toggle fastener (1.2) and sliding back the cooler, the insert can be installed. By this
means the heat is transferred linearly from the heater, though an insert, to the cooler
Heater
The heater (1.1) comprises external insulation, lid, brass rod and the electrical heater element.
There are three temperature measuring points under the insulation in the brass rod at 45.
Together with the insert there is thus a measurement section of nine measuring points.
Cooler
The cooler (1.4) comprises external insulation and a brass rod as for the heater. However this
brass rod has bores through which the cooling water can flow.
23
Inserts
Insert 1 (3.1) has three temperature measuring points in a brass rod. This brass rod has the same
diameter as the heater (1.1) and the cooler (1.2). When using other inserts, insert 1 can be placed on one
side.
Insert 2 (3.2) also has the same diameter as the heater and the cooler, but is made from corrosion
resistant steel (13) and does not have any temperature measuring points.
Insert 3 (3.3) on the other hand has a smaller diameter and is again made from brass, it also has no
temperature measuring points.
Theory
Heat conduction is the transfer of heat from one part of the body at a higher temperature to another part
of the same body at a lower temperature or from one body at a higher temperature to another body at a
lower temperature in physical contact with it. The linear heat transfer through conduction follows Fourier
law of heat exchange.
In this experiment, two surfaces, a heated and a cooled surface are clamped tightly together and are in
good thermal contact. The two sections can be considered as a continuous homogenous sample of
uniform cross section and material.
24
Figure 2: Fouriers law for temperature Profile in linear heat conduction
According to Fouriers law of heat conduction, if a plane section of thickness x and constant area A
maintains a temperature difference T then the heat transfer rate per unit time by conduction through
the wall is found to be:

Or, =
Where,
=
=
Or, =
[1]
Where, C is a constant that will be examined at a later stage.
If the material of the wall is homogeneous and has a thermal conductivity then,

=
[2]
The negative sign follows thermodynamic convention in that heat transfer is normally considered positive
in the direction of temperature fall. However, for the purposes of the following illustrations the negative
sign will be ignored.
Thermal conductivity, k, is a physical property of the conducting materials. For many practical
applications, it is considered a constant. However, in case of solids, k is often assumed to change with
temperature (k= k0 (1+T))
25
Procedure
For Part A:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
Ensure that main switch is in off position (the digital displays should not be illuminated)
Turn the voltage controller anti-clockwise to set the AC voltage to minimum
Ensure that cold water supply and electrical supply are turned on at source.
Smear the faces of the heated and cooled sections with thermal conducting paste and clamp
them together without any intermediate section in place.
Schematically this produces a system as shown in Figure 1.
Turn on the main switch and digital display should illuminate. Set the temperature selector switch
to T1 to indicate the temperature of the heated end of the bar
Set the heater power of approximately 90 Watts and monitor Temperature T1, T2, T3, T6, T7, T8
until it reaches steady state.
Record steady state temperatures T1, T2, T3, T6, T7, T8, V and I.
Vary the heater power from 90V to 200V and recording corresponding steady state temperatures,
voltage and current (Take minimum 4 readings).
After completion bring the heater power to zero and shut down the system.
.
For Part B:
1. Three different intermediates (sample specimens) will be used one each of brass, aluminum and
steel (detail specification of these samples are given below).
2. Insert one / desired sample in the sample holder between the heating and cooled surfaces and
toggle up the screws after applying the heat conducting paste.
3. Now repeat the steps as described in part A by varying the voltage from 90 V to 20 (Take
minimum 4 readings).
4. After completion of the first specimen, change the sample and repeat same procedure for other
two samples
26
Results and Discussion

For part A
1. Calculate rate of heat transfer, Q for each experimental run
2. Calculate Thot and Tcold values for each experimental run
3. Calculate temperature gradient for heated and cooled sections for each experimental run
4. Calculate
for each experimental run and compare the constant values for each experimental
run. Comment on the differences if any.

5. Plot the temperature distribution (T vs x) for each experimental run and comment on features.
6.
7.
8.
9.
For part B
Calculate rate of heat transfer, Q for each experimental run
Calculate thermal conductivity for all three sections
Compare the k [k = (x.Q)/(T.A)] values for the sections. Comment on the differences if any.
Plot the temperature distribution (T vs x) for each experimental run and comment on features.
Test Sample dimensions given in Appendix C & Physical properties of water in Appendix D
27
Tabulation
Measuring point
Measured
Distance S in mm
1
2
3
4
5
6
7
8
9
Temperature in C
Temperature
difference in K
Calculated
Coefficient of
thermal conduction
in W/m.K
10
20
30
40
50
60
70
80
APPENDIX C : Additional Information and Data

Heating Section Dimension
1.
2.
3.
4.
5.
Type: Heater
Shape: Cylinder
Material: Brass; 25mm Diameter
Thermocouples T1,T2, T3 at 15mm spacing
Thermal Conductivity: Approx. 121W/m oK
Cooling Section Dimension

1.
2.
3.
4.
5.
Type: Cooler
Shape: Cylinder
Material: Brass; 25mm Diameter
Thermocouples T6,T7, T8 at 15mm spacing
Test Sample Dimensions

1.
2.
3.
4.
Sample
a.
b.
c.
Sample
a.
b.
Sample
a.
b.
Sample
a.
b.
# 1: Brass Intermediate specimen

Dimension: 25 mm x 30 mm (Diameter x Length )
Thermocouples T4,T5, at 15mm spacing centrally spaced along the length
# 2: Stainless Steel Intermediate specimen
# 3: Aluminum Intermediate specimen
Thermal Conductivity: Approx. 180 W/m oK
# 4: Reduced Diameter Brass Intermediate specimen
Thermal Conductivity: Approx. 121 W/m oK
28
Appendix D: Physical Properties of Water
Table 1: Specific Heat Capacities of Water (Cp kJ/kgK)

C
4.1274
4.2138
4.2104
4.2074
4.2045
4.2019
4.1996
4.1974
4.1954
4.1936
10
4.1919
4.1904
4.1890
4.1877
4.1866
4.1855
4.1846
4.1837
4.1829
4.1822
20
4.1816
4.1810
4.1805
4.1801
4.1797
4.1793
4.1790
4.1787
4.1785
4.1783
30
4.1782
4.1781
4.1780
4.1780
4.1779
4.1779
4.1780
4.1780
4.1781
4.1782
40
4.1783
4.1784
4.1786
4.1788
4.1789
4.1792
4.1794
4.1796
4.1799
4.1801
50
4.1804
4.1807
4.1811
4.1814
4.1817
4.1821
4.1825
4.1829
4.1833
4.1837
60
4.1841
4.1846
4.1850
4.1855
4.1860
4.1865
4.1871
4.1876
4.1882
4.1887
70
4.1893
4.1899
4.1905
4.1912
4.1918
4.1925
4.1932
4.1939
4.1946
4.1954
Table 2: Density of Water ( kg/m3)

C
999.8
999.9
999.9
999.9
999.9
10
999.7
999.5
999.2
998.9
998.6
20
998.2
997.8
997.3
996.8
996.2
30
995.7
995.0
994.4
993.7
993.0
40
992.2
991.4
990.6
989.8
988.9
50
988.0
987.1
986.2
985.2
984.2
60
983.2
982.2
981.1
980.0
978.9
70
977.8
976.6
975.4
974.2
973.0
29
EXPERIMENT
Radial Heat transfer
FOUR
FREE & FORCED CONVECTIVE HEAT TRANSFER

Introduction:
Introduction
This experiment is designed to demonstrate the fundamental of heat transfer by radial conduction
corresponds to the conduction through a hollow cylinder. While for a wall the cross sectional area of the
heat flow remains constant, the area though which the heat flows changes. The heat transfer will be
monitored using thermocouples which are separated by equal distance.
Figure 1: Temperature distribution in radial heat conduction heat transfer
30
Figure 2: Radial heat conduction apparatus
The WL 372 Heat Conduction Unit is a tabletop unit ( F i g u r e 2 ) with two experimental arrangements,
linear conduction (1) and radial conduction (2). The storage vessels serve as storage locations for the
inserts (3).The control and display unit (4) is placed near the study unit. The two units are connected
together via two cables, a data cable (5) and a power cable (6). Laboratory cooling water feed and
return system and mains power complete the experimental setup
Objectives:
The main objective of this experiment is as follows;
A. To plot the temperature distribution for the radial conduction.
B. Determination of thermal conductivity coefficient.
Radial Conduction
The setup for radial conduction is a sealed unit comprises of
- An insulating housing with lid
- A disc with heater and cooler as shown in figure 1.
The heater is fixed from below in the center of the brass disc. There is a copper pipe around the disc
through which the cooling water can flow.
There are six temperature measuring points as shown in figure 1 fitted in line that stretches radially
from the center to the circumference. Using this apparatus the heat is transferred radially from the
heater to the cooler.
31
Theory
Heat conduction is the transfer of heat from one part of the body at a higher temperature to another part
of the same body at a lower temperature or from one body at a higher temperature to another body at a
lower temperature in physical contact with it. The linear heat transfer through conduction follows Fourier
law of heat exchange.
In this experiment, two surfaces, a heated and a cooled surface are clamped tightly together and are in
good thermal contact. The two sections can be considered as a continuous homogenous sample of
uniform cross section and material.
Figure 3: Fouriers law for temperature Profile in linear heat conduction
According to Fouriers law of heat conduction, if a plane section of thickness x and constant area A
maintains a temperature difference T then the heat transfer rate per unit time by conduction through
the wall is found to be:

Or, =
Where,
=
=
Or, =
[1]
Where, C is a constant that will be examined at a later stage.
32
If the material of the wall is homogeneous and has a thermal conductivity then,

=
[2]
The negative sign follows thermodynamic convention in that heat transfer is normally considered positive
in the direction of temperature fall. However, for the purposes of the following illustrations the negative
sign will be ignored.
Thermal conductivity, k, is a physical property of the conducting materials. For many practical
applications, it is considered a constant. However, in case of solids, k is often assumed to change with
temperature (k= k0 (1+T))
Figure 4. Radial Heat conduction surface
Radial conduction corresponds to the conduction of heat through a hollow cylinder.Whilst for a
wall the cross-sectional area of the heat flow remains constant, the area through which the
heat flows changes in the case of radial heat transfer
A = f ( r)
However the flow of heat remains constant and at any point on the cylinder one obtains
33
With A = 2*r**L
L = length of the cylinder
This yields
By reorganising and integrating over the limits ri to ra one obtains the flow of heat through a
hollow cylindewr
Procedure
1.
2.
3.
4.
5.
6.
7.
8.
9.
Ensure that main switch is in off position (the digital displays should not be illuminated)
Turn the voltage controller anti-clockwise to set the AC voltage to minimum
Turn Ensure that cold water supply and electrical supply are turned on at source.
Schematically this produces a system as shown in Figure 1.
Turn on the main switch and digital display should illuminate. Set the temperature selector switch
to T1 to indicate the temperature of the heated end of the bar
Set the heater power of approximately 90 Watts and monitor Temperature T1, T2, T3, T6 until it
reaches steady state.
Record steady state temperatures T1, T2, T3, T6 V and I.
Vary the heater power from 90V to 150 V and recording corresponding steady state
temperatures, voltage and current (Take minimum 4 readings).
After completion bring the heater power to zero and shut down the system.
34
Tabulation
Measuring point
1
2
3
4
5
6
Measured
Distance S in mm
10
20
30
40
50
Temperature in C
Results and Discussion

1. Determination of thermal conductivity coefficient.
2. Plot the temperature distribution.
Appendix A: Physical Properties of Water
Table 1: Specific Heat Capacities of Water (Cp kJ/kgK)

C
4.1274
4.2138
4.2104
4.2074
4.2045
4.2019
4.1996
4.1974
4.1954
4.1936
10
4.1919
4.1904
4.1890
4.1877
4.1866
4.1855
4.1846
4.1837
4.1829
4.1822
20
4.1816
4.1810
4.1805
4.1801
4.1797
4.1793
4.1790
4.1787
4.1785
4.1783
30
4.1782
4.1781
4.1780
4.1780
4.1779
4.1779
4.1780
4.1780
4.1781
4.1782
40
4.1783
4.1784
4.1786
4.1788
4.1789
4.1792
4.1794
4.1796
4.1799
4.1801
50
4.1804
4.1807
4.1811
4.1814
4.1817
4.1821
4.1825
4.1829
4.1833
4.1837
60
4.1841
4.1846
4.1850
4.1855
4.1860
4.1865
4.1871
4.1876
4.1882
4.1887
70
4.1893
4.1899
4.1905
4.1912
4.1918
4.1925
4.1932
4.1939
4.1946
4.1954
35
Table 2: Density of Water ( kg/m3)

C
999.8
999.9
999.9
999.9
999.9
10
999.7
999.5
999.2
998.9
998.6
20
998.2
997.8
997.3
996.8
996.2
30
995.7
995.0
994.4
993.7
993.0
40
992.2
991.4
990.6
989.8
988.9
50
988.0
987.1
986.2
985.2
984.2
60
983.2
982.2
981.1
980.0
978.9
70
977.8
976.6
975.4
974.2
973.0
36
Section II
Mass Transfer
37
EXPERIMENT
FIVE
WETTED WALL COLUMN
1. INTRODUCTION
Mass transfer coefficients are extremely useful in the design and scale-up of a variety of chemical
engineering processes including distillation columns, gas absorbers, and strippers. In view of the
complexity of mass transfer, fundamental equations for mass transfer are rarely available, and empirical
methods, guided by dimensional analysis, are relied upon to give workable equations. This problem has
been approached using experimental devices in which the area of contact between phases is known and
where boundary-layer separation does not take place. A wetted wall column is one device of this type. A
schematic diagram of a miniature wetted wall column is shown in Figure 1.
N2 Outlet
Figure 1: Schematic Diagram of Wetted Wall Column Setup

38
The wetted wall column essentially consists of a vertical tube with the inside surface of the tube covered
with a continuous sheet of liquid. The liquid is contacted in a counter-current manner with a gas stream,
and concentrations and flow rates of both the liquid and gas streams entering and leaving the column can
(in principle) be readily measured. The liquid which comes in contact with flowing gas partially diffuses
into the gaseous stream by means of convective mass transfer. This process is commonly used in
examining the mass transfer between components in two phases because the wetted wall column, unlike
other mass transfer processes, has a well defined interfacial between the two phases. The surface area is
assumed to be that of the inner tube surface area provided the liquid flows in a smooth, thin and laminar
layer.
2. OBJECTIVES
The objectives of this experiment are as follows:
1. To measure the mass transfer coefficient (kc) for oxygen diffusing into water as a function of the
gas and liquid flow rates.
2. To determine the power-law relationship between the liquid film mass transfer coefficient.
3. To compare the experimental result for kc with the values predicted from the Penetration Theory
and the Vivian-Peaceman correlation;
4. To comment on differences between the experimental, theoretical, and correlated values.
3. PRINCIPLES & WORKING EQUATIONS:

Following assumptions are useful for this experiment;
1. Equilibrium at interface
2. Laminar flow of the liquid film
3. Liquid film control
Mass transfer coefficient can be related to flux using following expression;
kc =
N O2
[1]
C L
The molar flux in equation [1] can be calculated from the volumetric flow rate (Ql) of the fluid and the
difference in concentration of the solute in the liquid entering and leaving the column;
N O2 =
Ql (C out C in )
AMT
[2]
The log-mean concentration driving force is defined by the following equation:

39
C L =
C out C in
[3]
C * C in
ln *
C C out
For this experiment, the solute is oxygen and the solvent is water. The equilibrium or saturation
concentration for oxygen in water can be determined from equilibrium relationships (e.g. Henrys Law),
from correlations, and from oxygen solubility data given in Appendix.
The area for mass transfer is given by:
AMT = ( DT 2 )h
[4]
Assuming laminar flow, it can be shown that 2
=3
3
2g
[5]
The assumption of laminar flow is critical to this experiment. For flow of fluids down an inclined surface,
the Reynolds number is given by:
Re =
[6]
According to Bird 1 the following criteria apply:

Laminar flow without ripples (smooth surface): Re <4 to 25
Laminar flow with ripples: 4 to 25 < Re < 1000
Turbulent flow: Re > 1000
Under no conditions should data be taken when the flow of the water is in the turbulent regime, as the
mass transfer will be dominated by eddy diffusivity.
Dimensionless Correlations
Following correlation has been developed for gasses dissolving in liquids:
Sh = 0.433Sc
1/ 2
2 gh 3
2
1/ 6
0.4
[7]
This correlation is known as the Vivian-Peaceman correlation.

A theoretical value for the mass transfer coefficient can be obtained using Higbie penetration theory:
40
k c = 1.13
Dv
tT
[8]
The contact time can be estimated as follows:
tT =
h
vi
[9]
Since the film is in laminar flow, it can be shown that the interfacial velocity is the maximum velocity;
vi = v max =
g 2
2
[10]
For analysis of experimental data;

Sh Re n
L
[11a]
Or
K Z
L
4 n
)
[11b]
Thus, construction of a logarithmic graph of
K Z
L
with ReL ( Sh L vs. Re L ) for various flowrates of
oxygen (in form of air) a power law relationship can be determined and compared with the published
correlation (equation 7 and 8).
4. RESULTS & DATA ANALYSIS
1. At constant air flow rate, determine the effect of water flow rate on the mass transfer coefficient
for a wide range of water Reynolds numbers.
2. At constant water flow rate, determine the effect of air flow rate on the mass transfer coefficient.
3. Compare your experimental results with Vivian-Peaceman correlation and the Higbie Penetration
theory.
4. Prepare log-log plots of Sh vs. Re for various air flow rates and determine the power law
relationship, i.e. the exponent n in equation [11]. Compare and Comment on the experimentally
calculated value.
5. Estimate and comment on the errors involved
Note: Refer to Appendix E for nomenclature and specifications of Wetted Wall Column
41
Appendix F: Nomenclature and Technical Specification of Wetted Wall Column
Figure 1: Schematic of Wetted Wall Column

Nomenclature
kc = Liquid film mass transfer coefficient
NO2 = Molar flux of oxygen from the gas to the liquid phase
C L = Log-mean concentration driving force

Ql = Volumetric flow rate of the liquid (units of volume per time)
Cout = Molar concentration of solute in liquid stream leaving the column = % O2 Out x C**
Cin = Molar concentration of solute in liquid stream entering the column = % O2 Out x C**
AMT = Area for mass transfer
C* = Equilibrium concentration
42
DT = Inner diameter of the column = 3.16 cm

h = Height of the column = 90 cm
Material: Glass
= Thickness of the water sheet
= Mass flow rate of liquid/wetted perimeter
k h
Sh = Sherwood number = c
Dv
Dv = Diffusivity of oxygen in water = 2.5 x 10-9 m2/s
Sc = Schmidt number for the liquid =
Dv
tT = Theoretical contact time between the two phases.

vi = Velocity of the liquid at the interface
Deoxygenating column height: 1570mm
Deoxygenating column internal diameter: 26mm
Deoxygenating column material: clear acrylic
Table:
Oxygen Solubility in Water (C*)
Temperature
(o C)
0
5
8
10
12
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
Solubility in Pure Water

(mg/l)
14.59
12.75
11.82
11.27
10.75
10.28
10.07
9.85
9.64
9.44
9.25
9.07
8.90
8.73
8.55
8.40
8.24
8.08
7.94
7.80
7.66
7.54
7.41
43
32
33
34
35
7.28
7.15
7.04
6.93
44
EXPERIMENT
SIX
MASS TRANSFER IN A PACKED COLUMN
1. INTRODUCTION
Packed columns are widely used in industrial mass-transfer operations, including adsorption, ion exchange and
various gas phase reactions. Gas absorption is a mass transfer operation in which a gas mixture is contacted
with a liquid to preferentially absorb one or more of the components of the stream. These towers are vertical
columns that have been filled with suitable packing. It involves a continuous countercurrent contact of two
immiscible phases. Fresh or regenerated liquid adsorbent is fed from top and falls by gravity. Liquid flows
downward while contacting with the vapor phase. Internal packing provides a large surface area for two-phase
contact and facilitates transfer of materials between phases. In this experiment glass Raschig rings are used as
packing materials. The liquid is distributed over the packing and flows down the packing surface as thin films
or subdivided streams. The progress of the mass transfer between the gas and liquid could be followed by
determining the amount of gas absorbed into the liquid.
2. THEORETICAL BACKGROUND
For a dry tower differential pressure drop (P) is related to the gas velocity (V) by an equation of the form:
P V n
[1]
The pressure drop is largely independent of the tower diameter, but it depends significantly on the nature of
the packing.
The introduction of liquid into the tower increases the frictional resistance and viscous drag affecting gas flow
and so the pressure drop is greater in the wet tower than in the dry tower. If the gas flowrate remains constant,
the pressure drop will increase with an increase in the liquid flowrate. This occurs because as the liquid fills the
voids in the column, the cross-sectional area available for gas flow is reduced. Up to the loading point, the
pressure drop graphs (P vs. V) at constant liquid rate show slopes that are fairly linear and approximately
equal to that of the dry run. Above the loading point, an increase in slope occurs, indicating a more rapidly
increasing pressure drop with increasing gas velocity. This continues until gas can no longer pass freely up the
column or the liquid pass freely down it. The frictional drag becomes so great that the downward flow of
liquid is substantially impeded and the column is to flood. At the flooding point, the slope becomes exponential
and the drag force of the gas bubbling through the down coming liquid is the predominate cause of the
pressure drop (Pflood) across the column [1-3].
45
Typical flooding curves are shown in McCabe et al., Figure 22.4 [1]. This graph has an abscissa of G (air mass
velocity) and an ordinate of P/Z (pressure drop per packing height). For two-phase flow through a packed
column, pressure drop correlations are graphed in various forms in McCabe et al., Figure 22.6.
Height equation for packed column absorption is given by:
H=
G MG
dy
K y .a. y * y
[2]
Figure 1: Schematic Diagram of the Gas Absorption Column
46
In order to integrate these equations over the column, it is necessary to determine the relationship between the
driving force (y-y*) or (p-p*) and gas or liquid composition. For a dilute gas, the above equation can be
simplified by considering the mean driving force for the whole column equals to the logarithmic mean of
concentration or partial pressure at the top and bottom. Therefore, the expression of the overall gas phase
mass transfer coefficient is;
ln
Ky =
pi
pO
G MG
x
a.H ( pi pO )
[3]
where, GMG = Molar Mass velocity of CO2 absorption (moles/cross sectional area. second)
3. DESCRIPTION OF EQUIPMENT
The Electroveneta gas absorption column has been designed to allow studying the hydrodynamic
characteristics either in the presence or absence of mass transfer process involving gas absorption. The column
is made of two 75 mm diameter borosilicate glass sections joined end to end to give a total column length of
1.4 m. The column is filled with 10 mm x 10 mm Rasching rings, which are representative of the type of
packing used in gas absorption. The liquid for the process is normally water and is stored in a 50 liter
rectangular sump tank. A centrifugal pump is used to deliver the liquid to the top of the column. A variable
area flowmeter F1 gives a direct reading of the liquid flowrate entering the top of the column. The flow of liquid
can be varied using the control valve V3. The gas to be absorbed is CO2 and would be taken from a cylinder of
compressed gas, located in a suitable storage rack adjacent to the column. The gas passes through a calibrated
variable area flowmeter F3 and is mixed with an air stream, also via a calibrated variable area flowmeter F2. The
flow of air can be varied using the control valve C2 above the air flowmeter. The ratio of gas to air in the
mixture entering the column is therefore known and easily varied. Tappings with an isolating valve are provided
at the base, centre and top of the column to allow indication of pressure drop in the two sections of column
using a pair of 'U' tube manometers. These tappings also provide a means of extracting samples of gas from the
column for analysis using the sampling syringe. The CO2 content of the gas samples is determined using a
Hempl apparatus and readings are indicated on the scale. A sampling point below the column allows analysis of
the liquid outlet stream. A sampling pipette S5 can be used to withdraw a sample of liquid from the sump tank
for analysis. The effluent gas leaves the top of the column via a cap with an overflow arrangement.
4. OBJECTIVES
1.
To study the effect of gas flow rate on the differential column pressure.
2.
To study the influence of the liquid and gas flow rates on differential column pressure.
3.
To measure the absorption rate of CO2 into H2O using the gas analysis.
5. RESULT & DATA ANALYSIS

47
1. Pressure differential should be plotted as a function of air flow rate on log-log graph paper to establish
the relationship between these variables for each water flow rate. The slope of the line is the exponent
of the power law correlation ( P V n ). This equation is valid for two-phase counter-current flow in
the packed tower from dry bed conditions to the loading point. Comment on the value of n obtained.
2. Calculate the mole fraction and amount of CO2 absorbed in the column from gas analysis of samples
at inlet and outlet.
3. Calculate the overall mass transfer coefficient (Ky) for each set of flow rates.
4. Estimate and comment on the errors involved
Note: For nomenclature refer to Appendix F
Appendix F: Nomenclature and Gas Analysis Procedure for G-L Absorption Column
Nomenclature
a
= Effective interfacial area per unit packed column (cm-1)
A = Cross sectional area of the tower (m2)

Z = Packing Height (m)
F
= Flow (litres/second)
G = Gas flow rate (g.moles/second)

V = Superficial gas velocity [volumetric flowrate (m3 /sec)/tower cross sectional area (m2)]
Kog = Gas-side mass transfer coefficient (g.moles/second.cm2.atm)
L
= Liquid flow (litre/second)
= Pressure (atm)
= Partial pressure (atm) = Y x P
= Mass transfer rate (g.moles/cm2.second)
VB = Volume of alkali solution added in liquid analysis (ml)

V1 = Volume of gas sample taken in Hempl apparatus (ml)
V2 = Corresponds to amount of gas absorbed in Hempl apparatus (ml)
X = Mole fraction of component in liquid phase
Y = Mole fraction of component in gas phase
Subscripts
i
= Inlet conditions to column
= Outlet conditions to column
N = Rate of CO2 absorption (g.moles/second)
48
Gas Analysis:
Start the pump G1 and adjust the flow rate of water to 200 L/h
Start the compressor P1 and adjust the flow rate pf air to approx.. 30 L/min
Open the micrometric valve of F12 and adjust the flow rate of CO2 to approx. 15 L/min
After 15 minutes extract a sample of gas from the top and from the center of the column and
analyze their content of CO2 complying with the directions specified here below.
Flux the sampling lines by sucking ( figure 2) and expelling (figure 3) the content of the syringe
into the environment. The volume of the syringe is of 100 ml, determine how many times this
operation must be repeated.
Figure 2
Figure 3
49
The figure above shows how gas can be intaken from the column bottom of course the valve V7
must be kept open. The gas available in the column top can be analyzed when the key of the valve
3V9 is turned upwards and those of the valves V10 and V11 are positioned horizontally.
The gas available in the center of the column can be analyzed when the key of the valve V10 is
turned upwards ad those of the valve V9 and V11 are positioned horizontally of course the valve
V8 must be kept open.
After insulating the globes and closing the vent to the outside ( figure 4) intake 20 ml of gas (V1)
with the syringe slowly then wait approximately 2 minutes until the gas reaches the syringe
temperature.
Figure 4
Insulate the syringe from the globes and from the column and balance the pressure with the
environment (Key for the valve V13 downwards). Close after approximately 10 seconds (key of
the valve V13 upwards).
Connect the syringe with the globes ( figure 5) . The level of the liquid should not vary otherwise
open to the outside environment for short time.
50
Figure 5
Wait until the level of the measuring hose coincides with zero thus indicating that the syringe
pressure is equal to the atmospheric pressure.
Push the syringe piston slowly to inject its content into the globes stopping when the solution of
NaOH tends to flow out of the right globe.
Pull the piston slowly up to its original position
Record the level of the measuring hose.
Repeat the operation unitl the level in the measuring hose does not undergo any great variation.
This value represents the volume of the sampling gas ( V2)
N.B : if the concentration of CO2 in the sampling gas exceeds 8% a part of liquid could be intaken by
syringe. In this case never try to draw the piston from the syringe , but keep a certain volume ( eg 20 ml)
and read the value indicated on the scale of the measuring hose.
51
EXPERIMENT
SEVEN
LIQUID LIQUID EXTRACTION
1. INTRODUCTION
Many processes in chemical engineering require the separation of one or more of the components of a liquid
mixture by treating the mixture with an immiscible solvent in which these components are preferentially
soluble. Liquid-liquid extraction is a mass transfer operation where a liquid solution (feed) is contacted with an
immiscible liquid (the solvent) in order to extract a desired component (solute). The solutions are not initially at
equilibrium with respect to the solute. Therefore, the solute will transfer from one phase (raffinate) to the
second phase (extract). The extract is rich in solvent containing the desired solute, and the raffinate is residual
feed solution, which has lost the solute due to extraction. Extraction is primarily used when distillation is
impractical or too expensive to use. It is the preferred mode of separation for heat-sensitive, high boiling, nonvolatile materials or compounds with comparable relative volatilities. The rate at which a soluble component is
transferred from one solvent to another will be dependent, amongst other things on the area of the interface
between the two immiscible liquids. Therefore it is very advantageous for this interface to be formed by
droplets and films, the situation being analogous to that existing in packed distillation columns. The major
disadvantage of the extraction process is the addition of a second separation stage to the process. This
additional stage is provided to recover the solvent from the solute and bring it back to the cycle. Extraction is a
commonly used unit operation in chemical, pharmaceutical, food, nuclear and oil industry. Important
applications in the petroleum industry include the separation of aromatic and aliphatic hydrocarbons.
The Armfield UOP5 LLE unit could be operated either by filling the column with water and allowing an
organic solvent to flow down the column, or filling the column with organic solvent and allowing water to flow
up the column. In either case the process is continuous. Sensing electrodes at the top and bottom of the
column determine whether the column is filled with water or with the organic solvent. This is achieved by
sensing and maintaining the position of the water level at the appropriate height. A solenoid valve controlling
the flow of solvent under gravity from the column is operated by the sensing electrode system. Organic solvent
could be recovered by employing the fractionating column.
A schematic diagram of the set-up is shown in Figure. The equipment, mounted in a floor standing, welded
steel framework, consists of a glass liquid-liquid extraction column (height=1.2 m, diameter=50 mm) packed
52
with Raschig rings of glass (10x10 size, inside diameter 8 mm). Water for the extraction column is pumped
from a supply tank via a flow control valve and flowmeter to an injector in the base of the column and flows
from an outlet pipe at the top to a collection tank. The organic solvent is pumped to the top of the column via
a metering pump and flow counter-current to the water supply. A sampling and drain cock is fitted in the
solvent feed line. A 3-way valve at the discharge of the solvent pump allows the flow from the pump to be
collected in a calibrated vessel for pump calibration. Solvent from the base of the column is returned under
gravity to the receiver vessel which is also fitted with a solenoid valve and a sampling cock. The level of the
water/solvent interface in the column is determined by the operation of the solenoid valve in the solvent outlet
pipeline. The operation of this valve is controlled by water-sensing electrodes, one set fitted to the top plate
and another set to the bottom plate. A switch on the system control panel selects the electrodes in use and
hence determines whether the interface is at the top or bottom of the column. The receiver vessel may be
connected to the solvent supply vessel for treating in a batch wise fashion or solvent could be re-circulated
continuously. The distillation column boiler mounted behind the extraction column, is fitted at such a height
that liquid may be drained into it from the upper of the three solvent tanks and can be drained from it into the
lowest tank. The valve controls the release of solvent into the boiler.
Figure 1: Diagram of UOP5 Liquid - Liquid Extraction Unit
53
3. OBJECTIVES
1. To generate equilibrium data for propionic acid-trichloroethylene-water system using batch extraction
process.
2. To demonstrate the continuous liquid-liquid extraction of propionic acid-trichloroethylene-water
system in a counter-current packed tower.
3. To perform mass balances on the extraction column.
4. To determine the overall mass transfer coefficient.
5. To calculate the height of transfer units, number of transfer units and the height of packing for
extraction.

Part A. Batch Extraction (Equilibrium Data)
1. Calculate propionic acid concentration in the extract (aqueous) phase, Y.
2. Calculate propionic acid concentration in the raffinate (organic) phase, X.
3. Draw the equilibrium curve (Y versus X) and draw a best fit straight line through the data, forcing
it to go through the origin.
Part B. Continuous Extraction

o
Construct the operating line (a straight line connecting (XY)top and (XY)bottom and the equilibrium curve on
the same figure.
Calculate the volumetric mass transfer coefficient, Ka, where;
Ka =
rate of propionic acid transfer

(volume of packing )(mean driving force)
(Y - Y )
*
Mean driving force =
top
(Y - Y * )bottom
(Y - Y )
(Y - Y )
*
ln
top
bottom
(X - X )
*
or
top
X - X*
(X - X )
(X - X )
*
ln
bottom
top
bottom
where X* is the concentration in the raffinate phase which is in equilibrium with Y value in the extract phase
and Y* that in equilibrium with X.
Rate of propionic acid from the organic phase (raffinate) = Raffinate flowrate x (Xtop-Xbottom)
o
Calculate the overall number of raffinate transfer units, NtOR or the overall number of extract transfer
units, NtOE.
54
Calculate the overall raffinate height of transfer units, HtOR or the overall extract height of transfer units,
HtOE.
Calculate the height of packing, Z and compare with the actual value (1.2 m).
Where, Z = HtOR NtOR = HtOE NtOE

Estimate and comment on the errors involved
Note: For nomenclature and technical specifications refer to Appendix G given below
Appendix G: Nomenclature and Schematic of Liquid Liquid Extraction System

Nomenclature
a
= Effective interfacial area per unit packed column (cm-1)
H = Height of the transfer unit (m)

Z
= Height of the packing unit (m)
N = Number of the transfer unit (stages)

F
= Flow (milliliters/second)
K a = Volumetric mass transfer coefficient
Given Data
Molecular weight of trichloroethylene: 133
Molecular weight of Propionic acid: 74
55
EXPERIMENT
EIGHT
DISTILLATION
1. INTRODUCTION
Separation of complex mixtures into pure component is one of the most important applications of the
chemical engineering processes. One of the most commonly used unit operation for separation in chemical
processes include both batch and continuous distillation column. The operation of the distillation columns is
generally governed by hydrodynamics of the internals that are used to contact the vapor and liquid. The
operation of a sieve plate is shown schematically in Figure 1.
Figure 1: Operation of a Sieve Tray

The main function of the plate (or tray) is to bring the vapor and liquid into intimate contact so that the
streams leaving the stage are as close to equilibrium as is possible. A stage or tray that brings the liquid and
vapor into equilibrium is called ideal and is said to have an efficiency of 100 %. There are, however limits to
hydrodynamics on the stage that make efficient contacting difficult. In normal operation, the flowrate of vapor
through the holes of the sieve tray is sufficient to provide a seal so that liquid coming to the tray from the
stage above flows across the tray, over the weir, and down the downcomer to the next tray. At low vapor
velocities however, the flowrate of vapor through the holes in the sieve tray can be so low that liquid leaks
through the holes of the tray rather than flowing across the tray. This condition is known as weeping. At the
56
other limit, high vapor velocities can entertain liquid from one stage to the next, essentially by passing the stage
completely.
At extremely high vapor velocities no liquid flow down the column is possible; this condition is known as
flooding. Both weeping and flooding represent situations where the overall efficiency of the column would be
expected to be low. Some published data on tray efficiency as a function of vapor velocity is shown in the
following Figure 2.
Figure 2: Sieve Tray efficiency as Function of Vapor Velocity [2]

The purpose of the lab is to demonstrate the relationship between the column efficiency and vapor flowrate,
pressure drop and vapor flow rate. In addition this experiment is designed to explore the weeping and flooding
characteristics.
The Armfield UOP3CC continuous distillation column is a self-contained distillation facility consisting of two
interconnected units: a floor standing process unit and a bench-mounted control console. The distillation
column is mounted on a floor standing, welded tubular steel framework with four adjustable feet. The glass
columns consist of two section having eight sieve plates of 50 mm diameter. The columns are separated by a
central feed section and arranged vertically for counter-current vapour/liquid flow. The liquid seal on the final
plate in each section is achieved by U-tube. Feed mixture from either of the feed tanks can be pumped either to
the base, centre or top of the distillation column. The reboiler situated at the base of the column. Either batch
or continuous distillation can be carried out using this reboiler. In continuous operation, valve (V1) is open and
57
bottom product flows from the reboiler through the bottom product cooler to the bottom product tank. It is
possible to preheat the feed to the column by directing the feed through a spiral coil in the bottom product
cooler where heat is transferred from product leaving the reboiler at the boiling point. When feeding cold feed
directly to the column, the product from the reboiler is cooled in the bottom product cooler by circulating cold
water through the spiral coil. For batch operation, valve (V1) remains closed so that the reboiler can be filled
with the initial charge (10 L) of binary mixture. Vapour from the top of the column passes to a water-cooled,
coil-in-shell condenser, which may be fitted with an insulated jacket to allow heat balances to be carried out
(The insulated jacket should not be fitted to the condenser for normal operation.). Cooling water enters the
condenser at a regulated rate through a rotameter and the flowrate is controlled by diaphragm valve (V5). A
cooling water supply is connected to the inlet nozzle and serves also to operate the vacuum pump when
operation at reduced pressure is required. Water supply to the vacuum pump is controlled by valve (V14), which
must only be operated when valve (V5) is open.
Condensate is collected in a glass decanter (phase separator) which is by-passed for normal experiments by
opening valve (V10). When the decanter is in use (separation of two immiscible liquids as condensate), valve
(V10) is closed so that the overflow and underflow pipes inside the vessel, can take effect. With valve (V10)
open, condensate from the condenser outlet passes directly through the decanter to the inlet of the reflux ratio
control valve which is a 3-way solenoid operated valve. Depending on the setting of the reflux timers,
condensate is directed by the reflux valve either back to the top of the column or to the top product collecting
vessel. When directed to the column, the reflux passes through a U-seal where a valve (V3) can be used for
measuring boil-up rate or for draining the U-seal. The contents of the top product tank can be drained into the
reboiler for re-use via valve (V12). Temperatures within the system are monitored by fourteen thermocouple
sensors (T1 to T14) located at strategic positions in the system. T1 to T8 are located in the column and measure
the temperature of the liquid on each sieve plate. The total pressure drop across the column is indicated on a
U-tube manometer via appropriate tappings in the column fitted with isolating valves (V6) and (V7).
3. OBJECTIVES
This experiment has been designed to gain hands-on experience on batch and continuous distillation. The main
objectives of this experiment are as follows:
1. To calculate the minimum number of ideal stages required for a certain separation of a mixture of
cyclohexane and n-heptane by graphical (McCabe-Thiele) and analytical (Fenske equation) methods.
2. To obtain the operating lines for stripping and rectifying sections.
3. To determine the actual number of trays for a given composition.
4. To determine the overall efficiency of the distillation column as a function of vapor flowrate.
5. To measure the overall pressure drop through the column as a function of vapor flowrate.
58
6. To perform the overall energy balance on the distillation column and determine the heat loss across the
column and corresponding overall heat transfer coefficient.
7. To estimate the heat duty of the condenser.
4. THEORETICAL BACKGROUND
Cyclohexane-n-pentane system will be used for this experiment. Equilibrium data for the binary mixture can be
found in the Appendix. From the data it is clear that relative volatily for this mixture, i.e.
AB = y A / x A y / x , is nearly constant and an approximate value of the 1.7 can be used.

B
B
A. Minimum Number of Stages

The minimum number of stages required to obtain a given separation (xB & xD) can be determined by
both analytical and graphical methods. The graphical determination is done by the McCabe-Thiele
method, where the operating lines for the stripping and rectifying sections are coincident with the 45
line. It can be shown that the minimum number of plates is found when the column us operated under
total reflux. The values of xD and xB found at steady state can then be used to prepare McCabe-Thiele
diagram as shown in Figure 3.
Figure 3: McCabe-Thiele Diagram for Total Reflux

Analytically, Fenske equation given below can be used to calculate the minimum number of the theoretical
plates required for a given separation at total reflux;
ln
N min =
x D (1 x B )
x B (1 x D )
ln AB
[1]
59
Where, AB = the relative volatility of the species A with respect to species B, defined as;
AB =
yA / xA
yA / xA
=
y B / x B (1 y A ) /(1 x A )
[2]
B. Column Efficiency
The efficiency of a distillation column can be measured by any of the following three ways;
Overall efficiency
Local efficiency
Murphee efficiency
For this experiment, we will apply overall efficiency ( 0 ). The overall efficiency is defined as;
0 =
Ni
Na
[3]
Where, Na and Ni refers to the number of actual and ideal (theoretical stage) stages respectively.
The number of the ideal stages required to achieve a given separation can be found either graphically or
analytical as described above. One of the requirements for this experiment is to examine how the overall
efficiency varies with the vapor flow rate between the condition of weeping and flooding. To make this
correlation, we need a method to determine the vapor flow rate.
C. Vapor Flow rate

Vapor flow rate at steady state can be measured directly by opening valve V3 by diverting the distillate product
from reflux line into a graduated cylinder, and timing the volume rate of discharge. This procedure however,
has the disadvantage of upsetting the operation of the column by temporarily re-routing the reflux from the
column to collection vessel (the graduated cylinder). This will result in column deviating from steady state;
depending upon the length of the time required to collect the sample this deviation may be insignificant, or
could be very significant and hence result in erroneous readings. An alternate method for determining the
vapor flowrate is by using energy balance on the condenser. By energy (enthalpy) balance and assuming
negligible heat losses from the condenser and insignificant superheat of the vapor and subcooling of the
condensate;
QC = m w C pw (Two Twi ) = V mix
[4]
Where,
QC
= rate of energy removal from vapor (condenser duty)
mw
= mass flowrate of the cooling water running through the condenser
Cpw
= heat capacity of the cooling water
Twi
= temperature of cooling water into the condenser
60
Two
= temperature of cooling water out of the condenser
= vapor flowrate (moles/time)
mix
= latent heat of vaporization of condensate (kJ/mole, mixture property)
The mixture latent heat can be estimated by mole fraction averaging from the composition of distillate product
and pure component latent heats;
mix = cyclohexane xcyclohexane + n hep tan e x n hep tan e
[5]
Where, xi= mole fraction of species i

Pure component latent heats can be found in standard thermochemistry reference tables.
D. Pressure Drop
Pressure drop at each vapor flow rate can be easily measured using water manometer. When the column has
reached steady state operation, pressure drop can be measured by opening the isolation valve V6 and V7.
E. Number of Plates using the LEWIS-SOREL Method

Material balance on the top of the column;
Vn = Ln +1 + D
[6]
With respect to more volatile component (cyclohexane), this becomes,

ynVn = Ln +1 xn +1 + DxD
yn =
Ln +1
D
x n +1 +
xD
Vn
Vn
[7]
[8]
Since liquid overflow is constant, i.e. Ln = Ln +1

yn =
Ln
D
x n +1 +
xD
Vn
Vn
[9]
Material balance on the top of the column;
61
V m = Lm +1 W
[10]
With respect to more volatile component (cyclohexane), this becomes;

y mV m = Lm +1 x m +1 + WxW
[11]
Lm +1
W
x m +1 +
xW
Vm
Vm
[12]
ym =
Since liquid overflow is constant, i.e. Lm = Lm +1

ym =
Lm
W
x m +1 +
xW
Vm
Vw
[13]
Equations [8] and [12] combined with the equilibrium curve can be used to calculate the composition on the
various plates working from the condenser down to the still. The plate which has a composition nearest to that
of the feed should be used as the feed plate. Consequently the number of theoretical plates and position of
entry for the feed can be calculated.
F. Batch Column Heat Losses

Applying overall heat balance for the distillation unit;
QL = QR - QC
[14]
Where,
QL =Heat losses from the distillation unit
QR = Heat input to the reboiler
QC = Heat removed by the condenser
Heat loss from the distillation column equals to the sum of the heat losses through the column (QLC) and
reboiler (QLR). Therefore, QL can also be defined as:
QL= QLC + QLR
[15]
62
However, the reboiler in our experimental set up is very well insulated and it can be safely assumed that QLC =
0. In this case:
QL =QLC= UACW TCW
[16]
Where,
TCW = TC -Tair
[17]
U is the heat transfer coefficient, TC is average column temperature and ACW is surface area of column.
63
5. DATA RECORDING
A. Batch Distillation
Ambient temperature
Heater Power
(kW)
Cooling Water
Pressure
Distillate
Flowrate
Twi
Two
Drop
Flowrate
(ml/min)
(O C)
(O C)
(mm H2O)
(ml/min)
Temperature ( O C)
T1
T2
T3
T4
T5
T6
T7
Concentration
T8
T
Reboiler
T
Column
Distillate
(fraction)
Bottom
(fraction)
B. Continuous Distillation
Feed composition
Heater power
Reflux
Pressure
Cooling Water
ratio
Drop
(mm H2O)
% Cyclohexane
(kW)
Flow rate
Flowrate
Twi
Two
(ml/min)
(O
(O
C)
C)
Feed
(ml/min)
Distillate
(ml/min)
Temperature ( O C)
T1
T2
T3
T4
T5
T6
T7
Concentration
T8
Reboiler
Column
Distillate
(fraction)
64
Bottom
(fraction)

1. Determine the minimum number of stages required to obtain the given separation at each vapor
flow rate. This determination should be done by
i. Graphical
: McCabe Thiele method
ii. Analytical
: Fenske equation
2. Determine overall column efficiency at each vapor flow rate and plot column efficiency vs.
vapor flow rate.
3. Plot pressure drop vs. vapor flowrate graph.
4. Draw the stripping and enriching operating line.
5. Calculate the number of theoretical trays and feed tray location.
6. Estimate the overall heat transfer coefficient between distillation column and ambient air.
7. Estimate the condenser heat duty.
8. Estimate and comment on the errors involved.
Note : Refer to Appendix H; for nomenclature and technical specifications of Distillation Column
65
Appendix H: Nomenclature and Schematic of Distillation System

Nomenclature
xD = mole fraction of distillate
xD = mole fraction of distillate
QC = rate of energy removal from vapor

mw = mass flow rate
Cpw = heat capacity of the cooling water
Twi = temperature of cooling water into the condenser
Two = temperature of cooling water out of the condenser
V = vapor flow rate (moles/time)
mix = latent heat of vaporization of condensate (kJ/mole, mixture property)

Na , Ni = number of actual and ideal stages
T1 =Temperature of the top tray of distillation column
T2 =Temperature of the 2nd tray of column
T3 =Temperature of the 3rd tray of column
T4 =Temperature of 4th tray of column
T5 =Temperature of the 5th tray of column
T9 =Temperature of the liquid in reboiler
T10 =Temperature of the vapor leaving the column
T11 =Temperature at top tray of column
T12 =Temperature of cooling water entering condenser
T13 = Temperature of cooling water leaving condenser
T14 =Temperature of feed liquid from the feed tank
Data:
Boiling point of the cyclohexane
= 81 O C
Boiling point of the n-heptane
= 98 O C
Actual number of trays
=8
66
Surface area of distillation column =9.4 x 10-2 m2
Figure 1: Schematic Diagram of the UOP3CC Distillation Rig
67
Table I1: Vapor Liquid equilibrium data for Cyclohexane and n-Heptane at 104.25 kPa
Y
0.00
0.00
98.43
0.05
0.0802
97.33
1.6569
0.10
0.155
96.22
1.6614
0.15
0.2272
95.22
1.6658
0.20
0.2946
94.20
1.6702
0.25
0.3582
93.21
1.6744
0.30
0.4184
92.24
1.6787
0.35
0.4754
91.30
1.6828
0.40
0.5293
90.37
1.6869
0.45
0.5804
89.47
1.6909
0.50
0.6289
88.59
1.6949
0.55
0.6749
87.73
1.6987
0.60
0.7186
86.89
1.7025
0.65
0.7601
86.06
1.7063
0.70
0.7996
85.26
1.7100
0.75
0.8372
84.47
1.7136
0.80
0.8729
83.70
1.7171
0.85
0.9070
82.95
1.7205
0.90
0.9395
82.21
1.7239
0.95
0.9704
81.48
1.7272
1.00
1.00
80.77
Log = 0.218106 + 0.02405. X 3.9918 x10 3. X 2
kPa
.673
) = 7.013111 (t 1228
+ 225.825)
(For Cyclohexane)
kPa
.105
) = 7.025730 (t 1267
+ 216.772)
(For n-Heptane)
Log P
Log P
68

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STUDENT

CHEMICAL ENGINEERING LABII

THE PETROLEUM INSTITUTE

CHEG455: CHEMICAL ENGINEERING LAB II

Section I: Heat Transfer

2. Plate Heat Exchanger

3. Linear Heat Conduction

4. Radial Heat Transfer

Section II: Mass Transfer

7. Immiscible Liquid Liquid Extraction

8. Distillation of Cyclohexanen Heptane

CHEG455: CHEMICAL ENGINEERING LAB II

INTRODUCTION AND EQUIPMENT DESCRIPTION

A3. THEORY/ BACKGROUND

A3.1. Temperature Efficiency

CHEG455 CHEMICAL ENGINEERING LAB II

Reduction in hot fluid temperature T = T1 - T2

Increase in cold fluid temperature T

Heat power emitted from hot fluid Q = qm . (Cp) (T1 - T2)

Heat power absorbed by cold fluid, Qa = qmc.Cpc (T4 T3)

Heat power lost or gained, Qf = Qe Qa

Temperature change in stream

Temperature efficiency for hot fluid h =

Temperature efficiency for cold fluid c =

(b) Cocurrent Operation

CHEG455 CHEMICAL ENGINEERING LAB II

Increase in cold fluid temperature, Tcold =

Temperature efficiency for hot fluid, h =

Temperature efficiency for cold fluid, c =

Mean Temperature Efficiency, m =

A3.2. Overall Heat Transfer Coefficient

CHEG455 CHEMICAL ENGINEERING LAB II

Arithmetic mean diameter, d

Heat transmission length, L

Where, n = number of tubes

l, heat transmission length of each tube

Heat transmission area, A

Overall heat transfer coefficient, U =

A4. RESULT & DATA ANALYSIS

B3. THEORY/ BACKGROUND

B5. RESULT & DATA ANALYSIS

Operating the Heat Exchanger Unit

Observe all safety precautions

Set the main power switch to position 1 from 0

Check the water level in hot water tank

Open cold water feed at the cold water mains

Open the regulator for cold water (V2)

Open the regulator for hot water (V1)

Start the pump (P)

Switch on the heater

Observe the measured values. Wait until a steady state is reached

When the experiment is complete, first turn off the heater

Then stop the pump

Close the regulator valves V1 & V2

Close the cold water feed at the mains

Set the main switch to 0

CHEG455 CHEMICAL ENGINEERING LAB II

Heat transmission length

Specific heat capacity hot fluid

Specific heat capacity cold fluid

Hot fluid inlet /outlet temperature

Cold fluid inlet/outlet temperature