Department of Chemical Engineering

College of Engineering

Qatar University

CHME 325
Unit Operations Lab Laboratory Manual

Spring 2024
 Contents
Preface .............................................................................................................................. iii

General Safety in the Laboratory .................................................................................. iv

U1. Cooling Tower ......................................................................................................... 5

1. Introduction and Theory ...................................................................................... 5

2. Apparatus and procedure ................................................................................. 12
2.1 Apparatus ...................................................................................................... 12
2.2 Procedure ...................................................................................................... 14
3. Safety Aspects: ................................................................................................... 14
4. References .......................................................................................................... 15
5. Report Requirements .........................................Error! Bookmark not defined.
U2. Tray Dryer .............................................................................................................. 16

Objective .................................................................................................................. 16
Theory ...................................................................................................................... 16
Equipment Setup .................................................................................................... 17
Procedure ................................................................................................................ 19
Report requirement ................................................................................................ 20
U3. Distillation ............................................................................................................... 21

1. Objective .............................................................................................................. 21
2. Introduction and Theory .................................................................................... 21
3. Apparatus and procedure ................................................................................. 25
3.1 Apparatus ...................................................................................................... 25
3.2 Procedure ...................................................................................................... 27
4. Safety Aspects .................................................................................................... 29
5. References .......................................................................................................... 29
6. Appendix .............................................................................................................. 29
U4. Fixed and Fluidized Bed ...................................................................................... 31

Objective .................................................................................................................. 31
Introduction.............................................................................................................. 31
Theory ...................................................................................................................... 31
Equipment Setup .................................................................................................... 33
Procedure ................................................................................................................ 34
U5. Wetted Wall Gas Absorption ............................................................................... 35

Theory ...................................................................................................................... 35

i
 Equipment Setup .................................................................................................... 38
Procedure ................................................................................................................ 39
Report requirement ................................................................................................ 40
U6. Gas Absorption ..................................................................................................... 41

Theory ...................................................................................................................... 41
Equipment Setup .................................................................................................... 42
Procedure ................................................................................................................ 43
U7. Molecular Diffusion in Gases .............................................................................. 45

1. Objectives: ........................................................................................................... 45
2. Introduction:......................................................................................................... 45
3. Apparatus ............................................................................................................ 47
4. Safety Aspects: ................................................................................................... 49
5. References .......................................................................................................... 49

ii
 Preface

The Unit Operations Laboratory in the Department of Chemical Engineering

provides a promising setting to help chemical engineering students become better
engineering practitioners. They get hands on experience of working with laboratory
setups – the theories of which they studied in Mass Transfer I and Mass Transfer
II courses. This course helps to reinforce and enhance the understanding of mass
transfer, the fundamentals of unit operations and separation processes learned in
theoretical courses.
This is the third edition of the Chemical Engineering Laboratory II (CHME 325)
manual. This edition comes as a result of need to improve contents and better
organization of the 2nd edition in accordance with various suggestions received
from faculties and students. The lab safety, lab rule observations, and guidelines
for preparing laboratory reports are incorporated herein this edition.
It is hoped that with the latest modifications, students and instructors will find this
edition of the manual clear and easier to follow and use.
However, our target in future is to develop this laboratory further with new
experimental setups and further improvements in the laboratory manual. This is an
ongoing process. The continuous help and support of the Department of Chemical
Engineering and its faculties in preparing this manual is highly acknowledged.

iii
 General Safety in the Laboratory
General safety rules and regulations are explained during the LAB orientation
week. So it’s compulsory that students attend that positively to be aware of the
general safety procedures. Following point must be observed during laboratory
sessions:

1. There should not be any storage or consumption of food and beverages in

the lab.
2. Smoking is not allowed in the laboratory.
3. LAB coats must be worn at all times during the whole laboratory session.
4. Wearing boots that cover the whole of the feet is absolutely compulsory.
5. Students should be wearing safety glasses wherever applicable during
laboratory sessions.
6. Students should be wearing gloves (vinyl or rubber gloves) when handling
liquid chemicals. Technician or TA must be around when handling
chemicals, especially harmful chemicals.
7. Students should be aware of the place where First Aid box is kept, showers
baths, and emergency phone numbers. Students should know the location
and use of all emergency, protective and fire fighting equipment.
8. Students are not recommended to open gas cylinders (associated with
specific experiments); instead they ask for assistance of LAB technician.
9. Inhalation of gases or vapors should be avoided. Masks should be worn.
10. Students should practice good house keeping. Clean all thrash and dump
them in dustbins. Also the equipment must be returned to original state
when experiment is completed.
11. Equipment should not be left unattended. Permission must be taken from
TA if student have to leave the lab due to an emergency situation.
12. Inform TA or technician if any safety problem is encountered.
Any violations in safety rule observation will be noted and marks will be
deducted from ‘Lab rule observation and compliance’.

iv
 U1. Cooling Tower
Objectives

1) To study the practical operation of a small cooling tower under a range of

process conditions and to observe the water flow pattern and distribution.
2) Set up mass and energy balances.
3) To study the effect of cooling load on “Wet bulb approach”
4) To calculate the number of transfer units, and the height of transfer units.
5) To calculate the overall mass transfer coefficient.

1. Introduction and Theory

What is a Cooling Tower? What is the use of cooling tower?
Cooling towers are basically an open system direct contact heat exchanger which
is used to lower the temperature of circulating water (to original thermal condition)
for reuse in power plant condensers and other heat exchangers. When warm liquid
is brought in contact with unsaturated gas, part of the liquid is vaporized and the
liquid temperature drops. This cooling of the liquid is the purpose behind many
gas-liquid contact operations, especially air-water contacts. The purpose of a
cooling tower is to conserve cooling water by allowing the cooled water to be
reused many times.
Many chemical processes require utility water to lower the temperature of process
streams. As it passes through a heat exchanger, the temperature of cooling water
is elevated. Before this water can be used as a cooling utility again, its temperature
must be lowered. The most common unit used to accomplish this goal is a cooling
tower.

How a cooling tower works? A cooling tower in principle is a special type of packed
tower. The usual packing material is cypress wood, which is the most economical
tower filling that withstands the combined action of wind and water. The warm
water is admitted at the top of the tower and moves counter flow to the air. In the
tower, part of the water evaporates into the air, and sensible heat is transferred
from the warm water to the cooler air. Both processes reduce the temperature of
the water. Waste heat present in the warm water is rejected to the atmospheric
air through convection and evaporation heat transfer [Saravanan 2008]. Only
make-up water to replace that lost by evaporation is required to maintain the water
balance.

Types of Cooling Tower: Cooling towers falls into two main sub-divisions: natural
draft and mechanical draft. Natural draft designs use very large concrete chimneys
to introduce air through the media. Due to the tremendous size of these towers
(around 500 ft high and 400 ft in diameter at the base) they are generally used for
water flow rates above 200000 gal/min. Usually these types of towers are only
used by utility power stations. Mechanical draft cooling towers are much more
widely used. These towers utilize large fans to force air through circulated water.
The water falls downward over fill surfaces that help increase the contact time
between the water and the air. This helps to maximize heat transfer between the
two.

The driving force for evaporation is, very nearly, the difference between the vapor
pressure of the water and the vapor pressure it would have at the wet-bulb
temperature of the air. Obviously the water cannot be cooled to below the wet bulb
temperature. In practice the discharge temperature of the water will differ from the
wet bulb temperature. This difference in temperature is called the approach to wet
bulb.
If water from a cooling tower is to be used for process cooling, the design of the
cooling equipment must be based on the maximum expected temperature of the
cooling water. This in turn depends, not on the maximum dry bulb temperature of
the air, but on the maximum wet bulb temperature.
The traditional approach to determine the mass transfer coefficient is to describe
the column height as the product of a HTU (height of transfer unit) and NTU
(number of transfer units). The HTU can be thought of as describing the efficiency
of contacting and the NTU as the difficulty of separation.

Relevant Cooling Tower Terms:

Cooling Range:
This is the difference between the water temperature at entry to and exit from the
tower.

Cooling Load:
The rate at which heat is removed from the water. This may be expressed in kW,
Btu/h or kcal/h.

Make-up water:
It is the quantity of fresh water which must be supplied to the water circuit to make
up the losses due to evaporation

Approach to Wet Bulb:

The Approach to Wet Bulb is one of the important parameters in the testing,
specification, design and selection of the cooling tower. This is given by the
difference between the temperature of the water leaving the tower and the wet bulb
temperature of the incoming air.
In a cooling tower of infinite size and with adequate air flow, the water leaving the
tower will be at the wet bulb temperature of the incoming air. For this reason, the
difference between the temperature of the water leaving a cooling tower and the
local wet bulb temperature is an indication of the effectiveness of the cooling tower.

Cooling Tower Performance:

The performance of a cooling tower is affected by the following factors:
a) The air flow rate

6
 b) The water flow rate
c) The water temperature
d) The air temperature and humidity at inlet (particularly the wet bulb
temperature)
e) The type of packing used
f) The area and volume of packing

Theory:
Setting up Mass Balance:
Ideally, rate of evaporation observed from the volume of water decreased in the
tank is equal to the moisture content difference in the air leaving the tower and the
air entering the tower.
Mathematically,
m E = m SB − m SA
= m a (ω B − ω A )
 E is the water evaporation rate, m SB is the moisture content in the outlet
Where, m
air, m SA is the moisture content in the inlet air, m a is the mass flow rate of dry air.
ω B and ω A are the moisture content or humidity ratio at the exit and inlet for air
(this is estimated using the psychrometric chart and using the inlet and exit air dry
bulb and wet bulb temperatures).
There are some non-idealities. So m  E and m a (ω B − ω A ) are calculated separately,
and the error percentage has to be determined and possible sources of error
should be discussed.

Effect of cooling load on “Wet bulb approach”

In a cooling tower of infinite size and with adequate air flow, the water leaving the
tower will be at the wet bulb temperature of the incoming air. For this reason, the
difference between the temperature of the water leaving a cooling tower and the
local wet bulb temperature is an indication of the effectiveness of the cooling tower.
“Approach to wet bulb” = (t6 – t2)

Calculation for Humidification operations): From Reference book of Geankoplis:

We consider a packed water – cooling tower with air flowing upward and water countercurrently
downward in the tower. The total interfacial area between air and liquid phases is unknown since
the surface area of the packing is not equal to the interfacial area between the water droplets and
the air. Hence, we define a quatity a, defined as m2 of interfacial area per m3 volume of packed
section. This is combined with gas phase mass-transfer coefficient kG to give a volumetric
coefficient kG a. the process is carried out adiabatically and the various streams and conditions are
shown in the figure below:

7
 L = water flow, kg water/s . m2
TL = temperature of water, ºC or K
G = dry air flow, kg/s . m2
TG = temperature of air, ºC or K
H = humidity of air, kg water/kg dry air
Hy = enthalpy of air-water vapor mixture, J/kg dry air

The enthalpy Hy is calculated by the following equation in SI units:

Hy = cs (T-T0) + Hλ0 = (1.005 + 1.88H)103(T-0)+2.501 x 106H
The base temperature selected is 0ºC or 273 K.
Assuming that L is essentially constant and only a small amount is evaporated, we make a total
heat balance for the dashed-line box shown in the figure below, and obtain an operating line:
G(Hy – Hy1) = LcL(TL – TL1) (1)

Figure 1 Continuous counter current adiabatic water cooling

The heat capacity cL of the liquid is assumed constant at 4.187 x 103 J/kg.K. When a plot of Hy
versus TL is made, we obtain a straight line with a slope of LcL/G. Making an overall heat balance
over both ends of the tower,
G(Hy2 – Hy1) = LcL(TL2 – TL1) (2)
Again making a heat balance for the dz column height and neglecting sensible heat terms
compared to the latent heat,
LcL dTL = G dHy (3)
The total sensible heat transfer from the bulk liquid to the interface is:
LcL dTL = G dHy = hL a dz(TL - Ti) (4)
Where hLa is the liquid-phase volumetric heat transfer coefficient in W/m3.K and the Ti is the
interface temperature. For adiabatic mass transfer the rate of heat transfer due to the latent heat
in the water vapor being transferred can be obtained as:
qλ/A = MBkGaPλ0(Hi – HG)dz (5)
where qλ/A is in W/m2, MB is the molecular weight of air, kGa is the volumetric mass-transfer
coefficient in the gas in kg mol/s.M3.Pa, P is the atmospheric pressure in Pa, λ0 is the latent heat
of water in J/kg water, Hi is the humidity of the gas at the interface in kg water/kg dry air, and HG is

8
the humidity of the gas in the bulk gas phase in kg water/kg dry air. The rate of sensible heat
transfer in the gas is
qs/A = hG a (Ti – TG) dz (6)
where qs/A is in W/m2 and hG a is the volumetric heat transfer coefficient in the gas in W/m3.K.
From the figure equation 4 must be equal to the sum of equations 5 and 6.
G dHy = MBkGaPλ0(Hi – HG)dz + hG a (Ti – TG) dz (7)

From theory:
hG a
≅ cs (8)
M Bkya

Substituting PkGa for ky a,

hG a
≅ cs (9)
M B Pk G a

Substituting the above equation (9) into equation (7), and rearranging,
G dHy = MBkGaP dz [(cs Ti + λ0Hi) – (csTG + λ0HG)] (10)

Adding and subtracting csT0 inside the brackets

G dHy = MBkGaP dz [cs (Ti – T0) + λ0Hi – {cs(TG – T0) + λ0HG}] (11)

The terms inside the braces are (Hyi – Hy), and hence the above equation becomes
G dHy = MBkGaP dz (Hyi – Hy) (12)

Integrating,
z H y2
G dH y
∫0 dz = z =
M B k G aP ∫
H y1
H yi − H y (13)

Often, only an overall mass-transfer coefficient KGa is available, and the above equation becomes
Hy2
G dH y
z=
M B K G aP ∫
H y1
H ∗y − H y (14)

First, H versus T plot for saturated air is drawn. The value of H*y is determined by going vertically
from the value of Hy at point P up to the equilibrium line.

9
 Figure 2 Temperature enthalpy diagram and operating line for water-cooling tower

(In many cases the film coefficients kGa and hLa are not available. The few experimental data
available indicate that hLa is quite large and that the value of Hyi would approach that of H*y in
equation 3.)

Knowing the entering air conditions TG1 and H1, the enthalpy of this air Hy1 is
calculated. The point Hy1 and TL1 (leaving water temperature) is plotted in the figure
as a point on the operating line. The operating line is plotted with a slope of LcL/G
and ends at point TL2, which is the entering water temperature. This gives Hy2.
Point P represents Hy and TL on the operating line and point R represents H*y on
the equilibrium line. Hence, the vertical line RP or H*y – Hy represents the driving
force.
The driving force H*y – Hy is computed for various values of TL between TL1 and
TL2. Then by plotting 1/( H*y – Hy) versus Hy from Hy1 to Hy2, a graphical (or
numerical) integration is performed to obtain the value of the integral in equation
14. Then, experimental value of KGa can be obtained.

To calculate the number of transfer units, and the height of transfer

units.
The height of the tower is 0.48 m. To get the height of transfer unit; we first have
to calculate the number of transfer units, described earlier. The number of transfer
unit is the integration part of the equation below. This is solved using graphical
integration with the help of MATLAB.
z Hy2
G dH y
∫0 dz = z =
M B kG aP ∫
H y1
H *y − H y

10
First, the equilibrium line is drawn using the enthalpies of saturated air.

Table 1 Enthalpies of saturated air-water vapor mixtures

T sat H (kJ/kg)

10 29.29303884
12 34.10376263
14 39.27608266
16 44.8512605
18 50.87488807
20 57.39736974
22 64.47447474
24 72.16797359
26 80.54637491
28 89.68578291
30 99.67090051
32 110.5962088
34 122.5673614
36 135.7028407
38 150.1359381
40 166.0171316

Next, the operating line is drawn using the information of temperatures of inlet (TL1)
and outlet water(TL2), and the enthalpies of the air entering the column (Hy1) and
leaving the column (Hy2).
Next, value of 1/(H*y - Hy) is calculated at selected values of Hy in between Hy1 and Hy2. We
find the integration value using MATLAB to find the area under the curve (trapz
function):
So the number of transfer units is obtained from the integration.

Next, the height of transfer unit (HOG) is calculated. This is given by: HOG = z/NOG,
where z is the tower height (0.48 m), and NOG is the number of transfer units just
calculated.

Overall mass transfer coefficient:

The overall mass transfer coefficient is calculated using the following equation.
G
H OG =
M B K G aP
G
So this will give: KG a =
H OG M B P
G = dry air flow, kg/s . m2

11
Note: The dimension for the packing cross section is 0.15 m × 0.15 m. the height
of the packing is 0.6 m.

2. Apparatus and procedure

2.1 Apparatus

The Basic Water Cooling Tower is used to introduce to the students the
characteristics and construction of a mechanical draft cooling tower. This operates
with moderate air and water flows with 0.5, 1.0 or 1.5 kW cooling loads.

Figure 3 Schematic diagram of a cooling tower system

12
The operation of a Basic Water Cooling Tower is as follows:

Water Circuit

Figure 4 Water Circuit of EC1000V Cooling Tower

The heated water from the tank is transferred to the top of the tower by a water
pump, with the cold water collected at the bottom of the tower and fed back into
the tank. A level gauge is present on the hot side of the tank, which indicates the
amount of water in the tank, as well as the maximum water level. To ensure a
constant level of water in the tank, a float valve is installed, with water slowly fed
into the tank to stabilize the water level and temperature. This facilitates accurate
results and provides a consistent environment for the temperature controller.

The unit is fitted with a centrifugal pump. The pump switch is located on the main
frame. The pump circulates water from the water tank through a needle valve to
regulate flow rate to the top of the column. The water is sprayed into the column,
it then passes by gravity down through the packing in the
column and back into the drip tray below. The water flow rate can be changed
using the needle valve.

Air circuit
A centrifugal fan is fitted on the right hand side of the unit. Air passes vertically
down a circular inlet duct to the fan. The fan accelerates the air, turns it 90
degrees and forces it into the right hand (dry) end of the water tank and up
through the tower. A calibrated orifice at the top of the fan inlet duct works with
an air pressure sensor to measure the air flow rate through the column. (VDAS®
calculates this automatically).

Versatile Data Acquisition System (VDAS®)

The EC1000V features in-built data acquisition hardware that facilitates direct
connection to a computer via a provided micro-USB cable. This connection is
located on the right-hand edge of the control panel, thus eliminating the need for

13
extra hardware. Our VDAS® software is optimally compatible with the EC1000V,
providing a range of essential features such as automatic logging and calculation
of data, enhanced productivity, increased accuracy, creation of charts and tables,
data export for further processing, and psychrometric chart generation.

Column Column Column

type A type B type C
Nº of levels 8 8 8
Nº of sheets by level 19 10 10
Total surface m2 1,915 1,013 0.680
Height of packaging (mm) 650 650 650
Density 112,64 58 40,02
Area/volume (m-1)

2.2 Procedure
1. Check that the level of water in the water tank overflows the level switch.
2. Choose a temperature for the water in the tank and wait until it is reached.
3. Choose a flow for the airflow and wait some minutes until it is reached.
4. Choose a flow for the water flow and wait some minutes until it is reached.
5. Record the data.

3. Safety Aspects:
1. The COSHH (Control of Substances Hazardous to Health) regulations
(1988) - The equipment used for this experiment involves the use of water

14
 which under certain conditions can create a health hazard due to infection
by harmful micro-organisms. For example, the microscopic bacterium called
Legionella pneumophila will feed on any scale, rust, algae or sludge in water
and will breed rapidly if the temperature of water is between 20 and 45°C.
Any water containing this bacterium which is sprayed or splashed creating
air-borne droplets can produce a form of pneumonia called Legionnaires
Disease which is potentially fatal. So the precaution for this is to change the
water regularly and not allowed to stagnate.
2. The equipment operates from a mains voltage electrical supply. The
regulations applying to the operation of electrical equipment must be
observed by the user. To give increased operator protection, and Earth
Leakage Circuit Breaker (ELCB, alternatively called a Residual Current
Circuit Breaker or RCCB) is provided as an integral part of the equipment.
If through misuse or accident the equipment becomes electrically
dangerous, and ELCB will switch off the electrical supply and reduce the
severity of any electric shock received by an operator to a level which, under
normal circumstances, will not cause injury to that person.

4. References
1. Lab Manual – Course handout, Chemical Engineering Department, Qatar
University.
2. Geankoplis, C.J., Transport processes and Unit Operations, 3rd Ed.,
Prentice Hall India.
3. Instruction Manual – Basic Water Cooling Tower (10), Dec. 1999.

15
 U2. Tray Dryer
Objective

To produce a drying and a drying rate curve for a wet solid being dried with air of
fixed temperature and humidity.
Theory

Immediately after contact between the drying media (wet solid) and the drying
medium (hot air), the solid temperature adjusts until it reaches a steady state. If
the solid is initially very wet the surface is essentially covered in a thin film of
liquid which is considered to be unbound moisture. The solid temperature and
the rate of drying may increase or decrease to reach the steady state condition.
At steady state, the temperature of the wet solid surface is the wet bulb
temperature of the drying medium. Temperatures within the drying solid also tend
to equal the wet bulb temperature of the air. However, lag between the
movement of mass and heat result in some deviation. Once the media
temperatures reach the wet bulb temperature of the air, the temperatures of the
media and air become stable and the drying rate remains constant. This is the
“constant rate drying”. The moisture is transported to the surface of the media by
capillary forces and drying is limited only by the rate at which the heat is
supplied. This period ends when the solid reaches the critical moisture content.
The surface film of moisture over the solid has been reduced by evaporation to a
point where any further drying causes dry spots to appear on the solid
surface. Beyond the critical moisture content, the surface temperature of the
solid rises and the drying rate falls off rapidly. This is the “falling rate” period and
can last for a significantly longer time than the constant rate period. This holds
true even though the moisture removal may be less. The drying rate approaches
zero as the moisture content reaches equilibrium. This is the lowest moisture
content obtainable with the solid under the drying conditions used.

Figure 1: Typical Drying Curve

16
 Figure 2: Typical Drying Rate Curve
Useful equations

Where:
Ss (kg) = Mass of dry solid
= Change in moisture content
(h) = Time period
A (m2) = Drying area

Equipment Setup

The equipment comprises a square section air duct fabricated from stainless
steel with variable speed fan, and removable trays for solids drying.

17
 Figure 3: Tray Dryer (Armfield, UOP8 – MKII)

(1)Switch. (2)Latched side door. (3)Adjustable Louvre. (4)Feet. (5)Air velocity

transmitter. (6)Electric Heating Element. (7)Air (dry bulb) temperature and
relative humidity sensors. (8) Screen. (9)Axial fan impeller. (10)Mesh screen.
(11)Load cells. (12)Support frame for the sample trays. (13) Buffle.

Air is drawn into the duct by an electronic motor driven axial fan impeller. The air
flow rate is determined using an air velocity transmitter.
The heated air passes over a combined humidity and temperature sensor before
passing over the three drying trays. Air temperature and relative humidity are
continuously measured at two points before and after the trays. The wet bulb
temperature can be calculated from Psychrometric Chart.

18
Specifications
• The dimensions for each tray are 254mm x 304.8mm x 9.5mm.
• The cross-sectional dimension of the central duct section (where the drying
trays are positioned) is (0.328 m x 0.177 m) = 0.051 m2.

Procedure

A. Preparing the Experiment (Preheating & Zeroing load cells):

1. Make sure the unit is switched off and remove the three drying trays from
the UOP8-MKII and set aside.
2. Turn on the UOP8-MKII tray drier using the main switch on the drier and
also by clicking the “power on” button (so that it appears as ) on the
Armsoft software.
3. Adjust the fan speed to achieve an inlet air velocity of 0.6m/s.
4. Note the temperature of T1 on the mimic diagram and enter this
temperature as the ambient air temperature by clicking on the
button on the mimic diagram.
5. Open the heater PID ( ) and set to automatic with a set point of 55°C.
Be aware that you must choose the option Automatic from the PID menu.
Check that the preheat temperature sensor rises, then stabilizes
approximately at the set point temperature.
Note: Load cells typically take 15 minutes to reach operating
temperatures. During this time step 1 of the experiment can be carried out.
6. After 15 minutes, change the option mode on the PID heater to Manual and
return the empty drying trays onto the tray holder in the UOP8-MKII drier
and zero each load cell by clicking each zero button ( ) on the
Armsoft software. All weight readings should now equal approximately 0.0
g.
Note: Take care when returning drying trays into the UOP8-MKII drier as
the internals may be hot and harmful to touch.
- It's important to return the Heater control to Manual operation whilst the
side door opens in order to protect the initial conditions set on the tray.
7. Immediately after zeroing the load cells, remove the three drying trays from
the drier.
8. Ensure the side door is closed.

B. Starting The Experiment:

1. Distribute the drying material onto each drying tray.

2. Adjust the sampling configuration by clicking on the button from the top
menu and set the sampling operating to automatic, and set the sample
interval to 2 minute intervals.

19
 5. Place the loaded drying trays on to the tray holder and lock the side door
closed.
Note: Take care when placing the drying trays into the UOP8-MKII drier
as the internals may be hot and harmful to touch.
6. Record the total weight indicated (material and water).
7. Change the operation back to Automatic on the Heater PID menu.
8. Then select the icon to begin the data recording of the sensor readings
into the results table.
8. The end of drying occurs when there is no change in the total weight for 5
– 10 minutes.
11. When the end of drying has been confirmed from the graph, select the
icon to stop recording data.
C- Ending The Experiment:
1. Set the heater PID to “OFF” to begin cooling the equipment. When T2
reaches room temperature set the fan speed to 0%.
2. Switch the UOP8-MKII drier off using the main switch on the drier.
3. Remove the trays from the tray holders and return the dried material.
4. Return the trays back onto the tray holders and lock the side door closed.

Report requirement

(1) Calculate the total moisture content removed from the solid. Calculate the
free moisture content
(2) Plot the drying curve relating moisture content as a function of time. On
the secondary axis plot the temperature after the trays (T2). Find the
drying periods on this curve.
(3) Produce the drying rate vs. moisture content curve.
(4) Calculate the theoretical drying rate.
(5) Comment upon the results obtained and relate the curves to the
mechanism by which drying occurs.
a. What is the significance of the equilibrium moisture content?
b. If the results did not reflect that which the theory suggests, what
may have caused this discrepancy?
c. When the “critical moisture content” occurs, what happens to T2?

20
 U3. Distillation
1. Objective
1) To observe the operation of the steady-state distillation of a binary mixture
under continuous operation.
2) Determine the theoretical number of stages
3) Determine the efficiency
2. Introduction and Theory
Distillation is one of the most important industrial processes for separating the
different components (having different volatilities or boiling points) of a liquid
mixture to obtain products of desired purity. Distillation usually forms part of a
larger chemical process, and is thus referred to as a unit operation. Design and
operation of a distillation tower depends on the feed and desired products.
Laboratory scale distillation columns are needed to provide adequate practical
training for students and plant operators in a safe environment. They may also be
used to acquire process separation data for use in full-scale plant design.
In distillation (fractionation) a feed mixture of two or more components of different
volatilities is separated into two or more products whose compositions differ from
that of the feed. Most often, the feed is liquid or vapor-liquid mixture. The bottoms
product is almost always a liquid, but the distillate maybe a liquid or a vapor or
both.
Separation by distillation requires the following: (1) a second phase be formed so
that both liquid and vapor phases are present and can contact each other on each
stage within the separation column, (2) the volatilities of the components are
different so that they will partition between the two phases to different extents, and
(3) the two phases can be separated by gravity or other mechanical means.
Distillation differs from absorption or stripping in that the second phase is usually
created by thermal means (vaporization or condensation) rather than by
introduction of a second phase that may contain an additional component or
components not present in the feed mixture.
Commercially, distillation has a number of uses. It is used to separate crude oil
into more fractions for specific uses such as transport, power generation and
heating. Water is distilled to remove impurities, such as salt from sea water. Air is
distilled to separate its components - notably oxygen, nitrogen and argon - for
industrial use. Distillation of fermented solutions has been used since ancient times
to produce distilled beverages with a higher alcohol content.
There are two main kinds of distillation: Simple Distillation & Fractional distillation.
Fractional distillation is essentially the same as simple distillation except that a
fractionating column is placed between the boiling flask and the condenser. The
fractionating column is usually filled with a packing. Fractional distillation gives
better separation between the liquids because the stages in the fractionating
column provide "theoretical plates" on which the refluxing liquid can condense, re-
evaporate, and condense again, essentially distilling the mixture over and over.

21
 Figure 1 Simple Distillation Figure 2 Fractional Distillation

Industrial distillation is typically performed in large, vertical cylindrical columns

known as distillation towers or distillation columns with diameters ranging from
about 65 centimeters to 16 meters and heights ranging from about 6 meters to 90
meters or more. When the process feed has a diverse composition, as in distilling
crude oil, liquid outlets at intervals up the column allow for the withdrawal of
different fractions or products having different boiling points or boiling ranges. The
"lightest" products (those with the lowest boiling point) exit from the top of the
columns and the "heaviest" products (those with the highest boiling point) exit from
the bottom of the column and are often called the bottoms.
In a binary distillation, the aim is to produce from the feed a distillate, rich in the
light key and a bottom product rich in the heavy key component. The ease or
difficulty with which separation can be achieved depends on the relative volatility,
α, of the two components, where
α 1, 2 = K 1 / K 2
If the two components form ideal solutions and follow the ideal gas law in the
vapor phase, Raoult’s law applies to give
K 1 = P1 / P and K 2 = P2 / P
s s

So relative volatility is given simply by the ratio of vapor pressures, α 1, 2 = P1 / P2 ,

s s

and thus is a function only for temperature.

The relative volatility can be expressed in terms of equilibrium vapor and liquid
compositions from the definition of the K-value as Ki = yi/xi. For a binary mixture,
y /x y (1 − x1 )
α 1, 2 = 1 1 = 1
y 2 / x 2 x1 (1 − y1 )
Solving for y1,
α 1, 2 x1
y1 =
1 + x1 (α 1, 2 − 1)

22
The mixture of 95.6% ethanol and 4.4% water (percentage by weight) is an
azeotrope with a boiling point of 78.2 ºC.
(For information only: The ethanol-water azeotrope can be broken by the addition
of a small quantity of entrainer – benzene or cyclohexane. Sometimes a molecular
sieve is used to selectively absorb the water from the 95.6% ethanol solution.
Synthetic zeolite can be used for this purpose. Membranes can also be used to
separate ethanol and water. Separation using membrane is not based on vapor-
liquid equilibria.)

Determining the Theoretical Number of Stages not at Total Reflux – McCabe

Thiele Method

In 1925, McCabe and Thiele published an approximate graphical method for

combining the equilibrium curve with operating line curves to estimate for a given
binary-feed mixture and column operating pressure, the number of equilibrium
stages and the amount of reflux require for a desired separation of the feed. The
step by step calculation procedure is as follows:
• Draw the equilibrium curve for the two-component system (ethanol water in
this case) on a x-y plot. Equilibrium data can be found using Aspen Plus for
the system at 1 atm.
• Draw the diagonal y = x line.
• Plot the bottoms, feed, and distillate ethanol mole fractions along the y = x
line.
• Plot the q-line (feed condition line) at the mole fraction of the feed from the
diagonal line extending through the equilibrium curve. The q-line is the
moles of liquid produced per mole of feed.
The condition of the feed stream F entering the tower determines the
relation between the vapor Vm in the stripping section and Vn in the enriching
section, and also between Lm and Ln. if the feed is part liquid and part vapor,
the vapor will add to Vm to give Vn. ‘q’ is defined as
heat needed to vaporize1 mol of feed at entering conditions
q=
molar latent heat of vaporization of feed
If the feed enters at its bubble point, the numerator is the same as the
denominator and so q=1. (The equation of the q-line is given by
q x
y= x− F )
q −1 q −1
• Plot the enriching operating line. The enriching operating line is given by the
following equation:
L Dx D
y n +1 = n x n +
Vn +1 Vn +1
Another form of the above equation is:
R x
y n +1 = xn + D
R +1 R +1
where, R is the reflux ratio.
xD= mole fraction of desired product in the distillate

23
 xn is the liquid composition leaving the nth stage.
yn+1 is the mole fraction of A in Vn+1 (Vn+1 is molar flow rate of vapor
from tray n+1)
The enriching line equation is a straight line on a plot of vapor composition
versus liquid composition, and it relates the compositions of two streams passing
each other
• The stripping section line can be drawn between the points where the
enriching line intersects with the q-line and the point where xw meets the
diagonal line.
The equation stripping section operating line is
L Wx w
y m +1 = m x m −
Vm +1 Vm +1
• Draw the theoretical stages by starting at xD on the diagonal line, move
horizontal to the equilibrium line, and then vertically back to the enriching
operating line.
• Continue the process towards xw, switching to the stripping section line after
crossing the q-line till you meet xw. (The optimum feed plate is one which
crosses the q-line.)
• Count the number of theoretical stages, and then determine the overall
efficiency.

The Armfield range of laboratory distillation columns is designed to provide safe,

‘hands-on’ practical training, whilst at the same time allowing comprehensive study
of the classic methods of distillation practice.
An important feature is incorporated within the plate column, whereby the
temperature on each sieve tray is measured and displayed.
In this experiment we study the separation of a binary mixture of ethanol and water
by distillation in a continuous operation.
The equilibrium curve is drawn, thereafter feed line, the xD and xW is marked.
Thereafter we get the equation of enriching section.
R x
The form of the equation is y n +1 = xn + D .
R +1 R +1
x
The y-intercept of the line is D
R +1
So a straight line is drawn connecting the point xD and the intercept. This is line for
the enriching section. The q-line is drawn. In our case the feed is saturated liquid.
So q= 1. the stripping line is drawn connecting xW and the point of intersection of
q-line and enriching line. The stages are drawn next.
Theoretical # of stages
So the efficiency = η = × 100%
Actual # of stages

Also make a plot (as a separate study) of temperatures at different plates

versus plate number to see how temperatures vary along the column, and
discuss this observation during steady state).

24
3. Apparatus and procedure

3.1 Apparatus

The equipment is mounted on a floor standing, welded tubular steel framework

fitted with four adjustable feet. The equipment comprises of a 50 mm diameter
sieve plate column made up of two glass sections each containing four sieve
plates. The columns are separated by a central feed section and arranged
vertically for counter-current vapor/liquid flow. Also installed within the framework
are: reboiler, 5 liters feed tanks, a peristaltic type feed pump, condenser, bottom
and top product tanks, reflux valve, and all appropriate instrumentation.
The reboiler situated at the base of the column is manufactured from 316 stainless
steel and incorporates a flameproof immersion type heating element. Either batch
or continuous distillation can be carried out using this reboiler.
In continuous operation, valve (V1) is open and 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.
Feed mixture from the feed tanks is pumped by pump to the base, center or top of
the distillation column. The glass column incorporates a total of eight sieve plates
in two sections each containing 4 plates (mentioned earlier). Each plate
incorporates a weir and downcomer to create a liquid seal between successive
stages.
Vapor from the top of the column passes to a water-cooled, coil-in-shell condenser.
The shell of the condenser incorporates a pressure relief valve to protect the
system in the event of a blocked vent or cooling water failure. Cooling water enters
the condenser at a regulated rate through a rotameter and the flow rate is
controlled by a diaphragm valve.
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 drop across the column is indicated on a U-tube manometer via
appropriate tappings in the column fitted with isolating valves.

25
Figure 1 Apparatus – Armfield Distillation Column

26
 Figure 2 Schematic diagram for continuous distillation

3.2 Procedure

A. Sample preparation and charging:

1. Prepare about 20 mole% ethanol water solution.

2. Verify its concentration using the refractometer.
3. Charge the feed beaker with 5 liters of this solution.
4. Charge the reboiler with 10 liters of the same feed solution. So in effect you
need to prepare 15 liters of solution. Make sure that the filter cap on the top
of the reboiler is firmly placed.
B. Start-up of the apparatus:

5. Turn on the power to the control panel.

6. In the panel set the temperature selector switch to T9, the temperature in
the reboiler.
7. On the control panel turn the power controller turn the power controller for
the reboiler heating element fully anti-clockwise and switch the switch
turning on the power of the heating element to “power on” position. Another
red lamp will illuminate indicating that the heating element is ‘on’. Turn the
power controller clockwise until a reading of approximately 0.75 kW is

27
 obtained on the digital wattmeter. The contents of the reboiler will begin to
warm up and this can be observed on the temperature read-out meter.
(Vapor will begin to rise up the column and the progress of this can be
clearly observed by the increasing temperatures when switching the
temperature selector on T8, T7, T6, T5, T4, T3, T2 and T1. The vapor
formed as a result of temperature rise will enter the condenser and reappear
as droplets into the glass walled distillate receiver vessel. The distillate will
build up a small level in the receiver and eventually overflow to the reflux
regulator valve.)

C. Steady State operation at total reflux:

8. As condensate starts to form, open valve V5 admitting cooling water to the

condenser at a flow rate of approximately 3 liters/min. This rate may be
varied according to the temperature of water. If there is insufficient water
flow, some of the vapor will be uncondensed and emerge from the vent pipe
at the side of the unit in which case increase the water flow rate.
9. Start the experiment with total reflux, meaning all the vapor condensed
liquid will return to the column.
(The cool distillate will return to the top of the column and will cascade down
the trays forming a liquid level on the trays. The vapor “bubbles” through
this liquid. The system will reach an equilibrium condition when the
temperatures T1, T2, T3, T4, T5, T6, T7 and T8 have reached an average
steady temperature)

D. Operation at partial reflux:

10. Set the reflux ratio to 5:1, meaning 5 sec back to column and 1 sec to top
product receiver. Switch the reflux valve “on”.
(You should now hear a “click”, meaning the reflux valve is working. You
should also see condensed vapor flowing to the top product receiver)
11. When stabilized, the flow of feed (at the mid point onto tray 5) and the reflux
can be started at the same time.
(It is advisable to set the feed flow of 2 liters/hr)
12. As the flow into the column becomes established, more vapor will rise up
the column and appear as condensate in the distillate receiver. Allow this to
flow to the top product receiver.
13. After feeding approximately 3 liters take a sample of the overheads through
valve “V3”. Generally, when taking samples from the top, drain a
“discarding” sample of approximately 5 to 10 ml before taking the
representative sample in a sample glass. Preferably at the same time, a
sample of the bottom is taken through valve “V2” (CAUTION: THIS
SAMPLE IS HOT).
14. Take 3 samples each of top and bottom at 10 minutes interval. Record the
refractive index for all the samples.
15. Save the datas collected for temperatures at various plates during steady
state operation.

28
4. Safety Aspects
1. Ethanol is a mild skin irritant, so nitrile or latex gloves must be worn when
the potential for contact exists.
2. There is also an inhalant and ingestion hazard linked with ethanol. Due to
the nature of the experiment vapors will escape although the air circulation
should prevent inhalation of a significant amount of vapors. However, if eye
irritation, headache, dizziness or nausea occurs, leave the lab immediately
and inhale fresh air.
3. When removing the liquid or vapor samples, a nitrile or latex glove may be
worn due to the high temperature of the samples.
4. It is also advisable to wear glasses or goggles at all times during the
experiment.
5. The cooling water should be turned on before any heating element is turned
on to ensure that any vapor created is condensed.

5. References
1. Lab Manual – Course handout, Chemical Engineering Department, Qatar
University.
2. Instruction Manual – Continuous Distillation Column (19) May 2004.
3. McCabe, W. L., J. C. Smith, P. Harriott, Unit Operations of Chemical
Engineeering, McGraw Hill International Editions, 4th Ed.

6. Appendix
The following attachment is the data logging sheet will be used by the students to
enter the data at the time of the experiment.

29
The following data should be used for getting calibration curve to get molar
composition of ethanol in the solution.

Molar % Refractive
ethanol Index

0 1.3314
12 1.3500
24 1.3595
36 1.3631
48 1.3646
60 1.3649
72 1.3645
82 1.3637
92 1.3626
100 1.3615

The plot for the above data:

Plot of refractive Index vs ethanol concentration

1.3700

1.3650

1.3600

1.3550
Refractive Index

1.3500

1.3450

1.3400

1.3350

1.3300

1.3250
0 10 20 30 40 50 60 70 80 90 100
Ethanol mol %

30
 U4. Fixed and Fluidized Bed
Objective

1) To verify the Carman-Kozeny equation

2) To observe the onset of fluidisation and differentiate between the
characteristics of a fixed bed and a fluidised bed
3) To compare the predicted onset of fluidisation with the measured
pressure drop.
4) To determine the pressure drop (head loss) across the beds with different
particle sizes
5) To observe the onset of fluidisation and differentiate between the
characteristics of a fixed bed and a fluidised bed for both particle sizes.
6) To compare the onset of fluidisation between the two particle sizes.
7) To demonstrate the phenomena of liquefaction of solids.

Introduction
The upward flow of fluid through a bed of granular material is a situation
encountered both in nature and in industry. Natural occurrences include the
movement of ground water, the movement of crude petroleum or the movement
of natural gas through porous media. Industrial occurrences include operations
such as back-washing filters, ion-exchange processes, extraction of soluble
components from raw materials and certain types of chemical reactor.
It is well known that if the granules are loosely packed and the pressure drop due
to the flow through the bed is equivalent to the weight of the bed then the
phenomenon of fluidisation occurs. The fluidised state occurs naturally in so-
called 'quick sands' where an object on the surface of the sand will quickly sink
through the sand when an upward flow of water occurs through the sand The
high rate of solids mixing that accompanies fluidisation is utilised in various
industrial operations such as drying, coating, heat transfer and chemical reaction.

Theory
To predict the performance of a fluidised bed, it will be necessary to know the
Voidage of the granules used in the beds I.e. the ratio of the voids (spaces)
between the granules to the total volume.
The bed Voidage (porosity) ɛ can be determined using the following equation:

………(1)
The Voidage for glass beads is typically 0.4, Where the Particle density for the
glass beads (Ballotini) is 2500 kg/m3. In Particulate Fluidizing Bed, where the
fluid is liquid, The void fraction of the expanded bed.
𝑳𝑳(𝟏𝟏 − ɛ) = 𝑳𝑳𝒎𝒎 (𝟏𝟏 − 𝜺𝜺𝒎𝒎 ) ………(2)

31
 𝑳𝑳𝑴𝑴 (𝟏𝟏−𝜺𝜺𝑴𝑴 )
𝜺𝜺 = 𝟏𝟏 − ………(3)
𝑳𝑳
Where (L) is the expanded bed height, (𝐿𝐿𝑚𝑚 ) is the minimum bed height (i.e. Fixed
Bed), (ɛ) is the porosity of the expanded bed, (𝜀𝜀𝑚𝑚 ) is the porosity of minimum
bed height.

To determine the interstitial velocity

𝒗𝒗𝒔𝒔� 𝑸𝑸
𝒗𝒗 = 𝜺𝜺 (and) 𝒗𝒗𝒔𝒔 = �𝑨𝑨………(4)
Where 𝒗𝒗 is the interstitial velocity and 𝒗𝒗𝒔𝒔 is the superficial (empty tube) velocity,
A is the bed cross-sectional area (Bed diameter = 0.05 m).

To determine the porous medium friction factor

−∆𝑷𝑷−𝑳𝑳𝑳𝑳𝑳𝑳 𝒅𝒅 𝟏𝟏 𝜺𝜺𝟑𝟑
𝒇𝒇𝑷𝑷𝑷𝑷 = ∗ ∗ 𝟐𝟐 ∗ (𝟏𝟏−𝜺𝜺) ………(5)
𝝆𝝆 𝑳𝑳 𝒗𝒗𝒔𝒔

Where, 𝑑𝑑 is the size of granules (m) = 0.625 x 10-3 m for the larger granular
material, and 0.250 x 10-3 m for the smaller granular material.

To determine the porous medium Reynold Number

𝒅𝒅𝒗𝒗𝒔𝒔 𝝆𝝆
𝑵𝑵𝑹𝑹𝑹𝑹, 𝑷𝑷𝑷𝑷 = ………(6)
𝝁𝝁(𝟏𝟏−𝜺𝜺)
Where 𝜇𝜇 is the viscosity of water (10-3 Nsm-2)

To determine the theoretical friction loss in porous media, (Carman-Kozeny)

equation is applied
𝟏𝟏𝟏𝟏𝟏𝟏
𝒇𝒇𝑷𝑷𝑷𝑷 = ………(7)
𝑵𝑵𝑹𝑹𝑹𝑹, 𝑷𝑷𝑷𝑷

From equations (5) and (7) Pressure drop per unit length can be determined
theoretically, and Carman-Kozeny equation can be expressed in the form

𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏(𝟏𝟏−𝜺𝜺) ∆𝑷𝑷 𝒅𝒅 𝟏𝟏 𝜺𝜺𝟑𝟑

= ∗ ∗ 𝟐𝟐 ∗ (𝟏𝟏−𝜺𝜺) ………(8)
𝒅𝒅𝒗𝒗𝒔𝒔 𝝆𝝆 𝝆𝝆 𝑳𝑳 𝒗𝒗𝒔𝒔

∆𝑷𝑷 𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝒗𝒗𝒔𝒔 (𝟏𝟏−𝜺𝜺)𝟐𝟐 ∆𝑷𝑷 𝟏𝟏𝟏𝟏𝟏𝟏∗𝝆𝝆∗𝒗𝒗𝟐𝟐𝒔𝒔 (𝟏𝟏−𝜺𝜺)

= (or) = ………(9)
𝑳𝑳 𝒅𝒅𝟐𝟐 𝜺𝜺𝟑𝟑 𝑳𝑳 𝑵𝑵𝑹𝑹𝑹𝑹, 𝑷𝑷𝑷𝑷 ∗𝒅𝒅 𝜺𝜺𝟑𝟑

To determine the experimental permeability (k) of the porous media

∆𝑷𝑷 𝝁𝝁
= � � 𝒗𝒗𝒔𝒔 ………(10)
𝑳𝑳 𝒌𝒌
To determine the theoretical permeability (k) of the porous media, modified
(Carman-Kozeny) equation is applied as

32
 𝒅𝒅𝟐𝟐 𝜺𝜺𝟑𝟑
𝐊𝐊 = � � ………(11)
𝟏𝟏𝟏𝟏𝟏𝟏(𝟏𝟏−𝜺𝜺)𝟐𝟐

At Incipient fluidization (onset of fluidisation) the force due to pressure drop must
be equal to the weight of the bed.
𝑩𝑩𝑩𝑩𝑩𝑩 𝒘𝒘𝒘𝒘𝒘𝒘𝒘𝒘𝒘𝒘𝒘𝒘
−∆𝑷𝑷 = 𝑨𝑨
= 𝝆𝝆𝒔𝒔 (𝟏𝟏 − 𝜺𝜺)𝒈𝒈𝒈𝒈 + 𝝆𝝆𝝆𝝆𝝆𝝆𝝆𝝆 ………(12)

𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝒗𝒗𝒔𝒔 (𝟏𝟏−𝜺𝜺)𝟐𝟐
−∆𝑷𝑷 = = 𝒈𝒈𝒈𝒈[(𝝆𝝆𝒔𝒔 − 𝝆𝝆)(𝟏𝟏 − 𝜺𝜺)] ………(13)
𝒅𝒅𝟐𝟐 𝜺𝜺𝟑𝟑

To determine the minimum fluidization velocity

𝒈𝒈(𝝆𝝆𝒔𝒔 −𝝆𝝆)𝒅𝒅𝟐𝟐 𝜺𝜺𝟑𝟑𝒎𝒎
𝒗𝒗𝒎𝒎𝒎𝒎 = 𝟏𝟏𝟏𝟏𝟏𝟏𝟏𝟏(𝟏𝟏−𝜺𝜺𝒎𝒎 )
………(14)

Equipment Setup

The Armfield CEL-MKII is designed to facilitate the study of flow through fixed
and fluidised beds of solid granules. Low flow rates allow the characteristics of a
solid bed to be investigated. Increasing flow rates allow the onset of fluidisation
and the characteristics of a fluidised bed to be investigated.

33
 Figure 1: Fixed and Fluidised Bed Apparatus (Armfield CEL-MKII)

The CEL-MKII has three test columns, one for use with water and two for use
with air. With granules of the same size in the water column and one air column,
the differences between ‘particulate’ and ‘aggregative’ (‘bubbling’) fluidised beds
can be demonstrated. The two air columns allow the effect of different granule
sizes to be demonstrated without having to remove, empty and re-pack a
column.
Electronic instrumentation is incorporated, allowing all relevant flow rates and
differential pressures to be displayed. A USB connector allows the measured
variables to be viewed and logged on a PC if required using the software
supplied with CEL-MKII.

Specifications
• The bed cross-sectional area (Bed diameter = 0.05 m).
• The size of the granules (m) = 0.625 x 10-3 m for the larger granular
material, and 0.250 x 10-3 m for the smaller granular material.
• Voidage for glass beads is typically 0.4
• The particle density for the glass beads (Ballotini) is 2500 kg/m3.

Procedure

1) Set the flow regulator in front of the column to minimum flow (fully
anticlockwise).
2) Switch on the air compressor or water pump via the switch on the console.
3) Adjust the flow rate in increments of small quantities l/min by slowly
turning the flow regulator clockwise and observing the flow reading on
display.
4) Continue increasing the flow until the bed is fully fluidised and the
pressure drop across the bed remains constant for several readings.
5) At each setting allow the conditions to stabilize, then record the flow rate
and the differential pressure reading from the display.
6) Also record the height of the bed, measured using the scale on the
column, and observe and record the state of bed i.e. any movement of the
granules.

Report requirements.
Discuss the effect of particle size and fluid type on the pressure drop, friction
factor and minimum required velocity.

34
 U5. Wetted Wall Gas Absorption

Objective
1. To estimate the liquid film mass transfer coefficient.
2. To determine the power-law relationship between the liquid film mass
transfer coefficient and the mass flow rate of water and to compare the
results with theoretical predictions.
3. Discuss the effect of both liquid phase and gas phase flow rates on the
mass transfere coeffificent.

Theory
The process of absorption of gases in liquid in absorption towers is widely used
in industry. The process facilitates the removal of one or more components from
a mixture of gases. This is achieved by diffusion into a suitable liquid.
In view of the complexity of mass transfer in actual mass transfer devices such
as packed towers, sieve trays and bubble cap columns, fundamental equations
for mass transfer are rarely available. This problem has been approached using
experimental devices in which area of contact between the phases is known and
where boundary layer separation does not take place. Wetted wall column is one
such device [McCabe Smith].
Wetted wall gas absorption tower is a vertical column in which liquid flows down
while the gas flows upward in counter current motion. The liquid comes in contact
with the flowing gas by means of convective mass transfer to dissolve one or
more of the gas components. The wetted wall gas absorption column provides a
means of determining this coefficient and has been widely used in the
development of correlations for packed towers. Mass transfer in wetted wall
column involves well defined interfacial area between the 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.
The absorption of oxygen in water is an example in which most of the resistance
to mass transfer lies in the liquid phase. Many measurements of the mass
transfer coefficient have been developed for comparison between the mass
transfer coefficient and the mass flow rate of the liquid stream.
There are two mass transfer coefficients that are of interest to us in finding them
for applying mass transfer applications, which are called the overall mass
transfer coefficients for gas and liquid phases ‘KG’/’KL’ for linear equilibrium
curves, and can be calculated using these formulas:

1 1 𝑚𝑚 1 1 1
= + = +
𝐾𝐾𝐺𝐺 𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿 𝐾𝐾𝐿𝐿 𝑚𝑚𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿
Where,

35
‘𝐾𝐾𝐺𝐺 ’ is the overall mass transfer coefficient for gas phase.
‘𝐾𝐾𝐿𝐿 ’ is the overall mass transfer coefficient for the liquid phase.
‘𝑘𝑘𝐺𝐺 ’ is the gas film mass transfer coefficient.
‘𝑚𝑚’ is the proportionality constant for the linear equilibrium curves.

Two extremes can be extracted from the previous formulas;

(1) “Liquid phase controlled” system
Where the solubility of gas in liquid is very low (e.g. Oxygen in water), the value
of proportionality constant 𝑚𝑚 becomes very high and as a valid assumption the
gas phase resistance is ignored as illustrated here:

1 1 1 1 KLz
= + ≈ ⬄ ( Sh) L =
KL m𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿 𝑘𝑘𝐿𝐿 DL
1 1 𝑚𝑚 𝑚𝑚 mK G z
= + ≈ ⬄ ( Sh) L =
KG 𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿 𝑘𝑘𝐿𝐿 DL

(2) “Gas phase controlled” system

Where the solubility of gas in liquid is very high (e.g. Ammonia in water), the
value of proportionality constant 𝑚𝑚 becomes very small and as a valid
assumption the liquid phase resistance is ignored as illustrated here:

1 1 1 1
= + ≈
KL m𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿 m𝑘𝑘𝐺𝐺
1 1 𝑚𝑚 1
= + ≈
KG 𝑘𝑘𝐺𝐺 𝑘𝑘𝐿𝐿 𝑘𝑘𝐺𝐺

In the current experiment, the oxygen is dissolving in a deoxygenated water

(where the solubility of gas in liquid is low), the main assumption: The mass
transfer coefficient (K L ) is approximately equal to liquid film mass transfer
coefficient (𝑘𝑘𝐿𝐿 ).

The empirical Mass transfer correlations published in the literature.

(𝑆𝑆ℎ)𝐿𝐿 = 0.433 𝑆𝑆𝑆𝑆𝐿𝐿 0.5 𝐺𝐺𝐺𝐺𝐿𝐿 1/6 𝑅𝑅𝑅𝑅𝐿𝐿 0.4

Reynold’s Number Describes the ratio of Inertial 𝐷𝐷ℎ 𝑣𝑣𝑣𝑣

𝑅𝑅𝑅𝑅 =
(Re) forces to Viscous forces. 𝜇𝜇
Sherwood Number Describes the ratio of the Mass 𝑘𝑘𝐿𝐿 𝑧𝑧
𝑆𝑆ℎ =
(Sh) transfer rate to Mass diffusivity. 𝐷𝐷𝐿𝐿
𝜇𝜇
Schmidt Number • Describes the ratio of the �𝜌𝜌�
(Sc) Momentum diffusivity 𝑆𝑆𝑆𝑆 =
𝐷𝐷𝐿𝐿

36
 (kinematic viscosity) (ν=μ/𝜌𝜌)
to the Mass diffusivity.
• Is used to characterize fluid
flows in which there are
simultaneous momentum
and mass diffusion
convection processes.
• Describes the ratio of the
Gravity forces to viscous
forces.
Galileo Number • Is used in viscous flow and 𝜌𝜌2 𝑔𝑔𝑧𝑧 3
𝐺𝐺𝐺𝐺 =
(Ga) thermal expansion 𝜇𝜇 2
calculations, for example to
describe fluid film flow over
the walls.

Where
4A
Dh = hydraulic diameter, Dh = P
kL = liquid film mass transfer coefficient, ms-1
z = height of column, m
DL = diffusivity of oxygen in water, m2/s
µL = viscosity of water Ns/m2
ρL = density of water kg/m3
Γ = mass flow rate of water per meter of wetted perimeter kg/s-m

ScL and GaL are constants if the properties of fluid are not changing
(Temperature is assumed constant). It is therefore possible to determine the
power-law relationship between (Sh)L and (Re)L by experiment and compare it
with the above correlation.

Mass Transfer Coefficecnt can be determined form the following equation

𝑸𝑸 �𝐶𝐶𝑂𝑂2 (𝑜𝑜𝑜𝑜𝑜𝑜) − 𝐶𝐶𝑂𝑂2 (𝑖𝑖𝑖𝑖) �
𝑲𝑲𝑶𝑶𝑶𝑶 = ∗
𝑨𝑨 ∆𝑪𝑪𝑳𝑳𝑳𝑳
�𝐶𝐶𝑂𝑂∗2 − 𝑪𝑪𝑶𝑶𝟐𝟐 ,𝒊𝒊𝒊𝒊 � − �𝐶𝐶𝑂𝑂∗2 − 𝑪𝑪𝑶𝑶𝟐𝟐 ,𝑶𝑶𝑶𝑶𝑶𝑶 �
𝜟𝜟𝑪𝑪𝑳𝑳𝑳𝑳 =
�𝐶𝐶𝑂𝑂∗ − 𝑪𝑪𝑶𝑶𝟐𝟐 ,𝒊𝒊𝒊𝒊 �
𝒍𝒍𝒍𝒍 � ∗ 2 �
�𝐶𝐶𝑂𝑂2 − 𝑪𝑪𝑶𝑶𝟐𝟐 ,𝑶𝑶𝑶𝑶𝑶𝑶 �

Where
• 𝐾𝐾𝑂𝑂𝑂𝑂 :Overall Mass Transfere Coeifficent based on the Liquid phase
• 𝑄𝑄 is the volumentric flow rate (m3/s).
• 𝑨𝑨 is the area of mass transfer

37
 • �𝐶𝐶𝑂𝑂2,𝑂𝑂𝑂𝑂𝑂𝑂 − 𝐶𝐶𝑂𝑂2 ,𝑖𝑖𝑖𝑖 �Is the is the change in the oxygen concentration in the
water passing the column (mol/ m3).
• 𝛥𝛥𝐶𝐶𝐿𝐿𝐿𝐿 is the log mean concentration difference
• (𝐶𝐶𝑂𝑂𝐿𝐿2 ) is liquid phase oxygen concentration.
• 𝐶𝐶𝑂𝑂∗2 is the theoretical equilibrium oxygen concentration.

Equipment Setup

The Wetted wall gas absorption is a vertical column in which liquid flows down
while the gas flows upward in countercurrent motion. The liquid comes in contact
with flowing gas by means of Convective Mass Transfer to dissolve one or more
of the gas components. First, Water is sparged with nitrogen gas in order to
remove its oxygen content before entering the top of the wetted wall column.
Then, the Air is pumped by an air compressor into the base of the absorption
column. Air passes up the column, giving up the oxygen to the deoxygenated
water. The amount of dissolved oxygen at the inlet and outlet of the wetted wall
column can be measured using a DO calibrated electrode.

Figure 1: Wetted Wall Absorption Column (Pignat, France).

38
.
Figure 2: Schematic diagram of Wetted Wall Column (Pignat, France).

Specifications and useful data for calculations

• The column diameter is 32.4 mm, and its height is 850 mm.
• The Diffusivity (𝐷𝐷𝐿𝐿 ) (𝑚𝑚2 𝑠𝑠 −1) = 2.5E-09
• Gravity (𝑚𝑚𝑠𝑠 −2 )= 9.81
• 𝜌𝜌 (kg. 𝑚𝑚−3)= 997.64
• 𝜇𝜇 (kg. 𝑚𝑚−1 𝑠𝑠 −1 )= 1.008E-03

Procedure
C. Preparation of the Experiment:
(1) Open the valve of nitrogen gas (1 bar) and allow it to flow through the
WWC to remove any traces of 𝑂𝑂2.
(2) Open V7 (to allow the 𝑁𝑁2 flow into the system).
(3) Open V9 (to allow the 𝑁𝑁2 flow into the WWC).
(4) Close V8 (to prevent the 𝑁𝑁2 flow through DeOC).
(5) Close V11 (to prevent the 𝑁𝑁2 flow through Air compressor hoses ).
(6) Monitor the OX2 that measure the 𝑂𝑂2 (mg/L) of the outlet WWC until
reaches ≈1 mg/L. Now the WWC is almost free of Oxygen, so we can
close it and allow the N2 to pass through the DeOC.
(7) Close V9 (to stop the N2 flow into the WWC).
(8) Open V8 (to allow the N2 flow through DeOC).
(9) Switch on Pump 1 and adjust the water flowmeter at 20 L/h (to allow
the water to be de-oxygenated in the DeOC and been derived to the
WWC.

39
 (10) Ensure that all wetted wall of the column is wetted with water (if not,
you can pour some water at the top of the WWC to make the column
totally wetted by water..
(11) Monitor O2 concentration that connected to OX2 until reaches around
0.4 mg/L. Now, the system is ready to start the experiment.

D. Starting of the Experiment:

(1) Adjust the water flowmeter (at 20 L/h).
(2) Open V11 (to allow air flow into the WWC).
(3) Switch on Pump 3 and adjust the Air flowmeter (at 200 L/h).
(4) Wait about 10 minutes, and then record the 𝑶𝑶𝟐𝟐 concentration that
connected to OX1 and OX2.
(5) Study the effect of changing of water flowrate for flowrates 15, 10 and
5 L/h.

Report requirement
(1) Calculate the overall mass transfer coefficient 𝐾𝐾𝑂𝑂𝑂𝑂 experimentally.
(2) Determine Sherwood Number from the calculated mass transfer
coefficient.
(3) Determine Sherwood Number empirically.
(4) From empirical Sherwood, number calculate theoretical liquid film mass
transfer coefficient.
(5) Find and discuss the difference between experimental and empirical
findings.
(6) Plot a relation between log Sh vs log Re, and check the validity of the
empirical Sherwood Number.
(7) Discuss the effect of both liquid phase and gas phase flow rates on the
mass transfer coefficient.

40
 U6. Gas Absorption

Objective
1. To estimate the Loading and flooding points in the wet column.
2. To compare between the pressure drop trend betwwen dry column and
wet column.

Theory
Absorption is a basic operation of mass transfer that consists on the separation
of some components of a gaseous miscture by contact with an adequate solvent.
The packed tower, in which two liquids flowing in opposite directions enable a
chemical component to be transferred from one fluid phase to the other, occurs
in almost all chemical plants. This process of chemical component transfer can
be gas absorption, distillation, solvent extraction etc. As a Chemical engineer
(design engineer) we should have the knowledge of the characteristics of fluid
flow and of mass transfer in such towers. The Armfield Gas Absorption column is
designed to allow both these studies to be made.
Packed towers are vertical columns filled with suitable packing and normally
operate countercurrently. Liquid enters the top of the column and is distributed
over the top of the column packing via nozzles or distributor plates. 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.
For a dry tower the differential pressure drop (P) is related to the gas flowrate (Q)
(or velocity) (V) by an equation of the form:
P Qn
P Vn

The pressure drop depends significantly on the nature of the packing. Different
packings have different free cross-sectional areas. The free cross-sectional area
is related to the voidage ().
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 flow rate remains constant, the pressure
drop will increase with an increase in the liquid flow rate. 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, nor 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

41
exponential and the drag force of the gas bubbling through the downcoming
liquid is the predominate cause of the pressure drop (Pflood ) across the column
Equipment Setup

The gas absorption column It is formed by a cylindrical gass tube of 1400 mm

long and 75 mm of internal diameter. The filling of the column is made of 8 mm
glass Rasching rings, supported by a nylon perforated plate. The liquid feeds to
the column through its upper end using a glass difussion shower. That assures
an uniform distribution over the filler. Air is supplied by a blower that provides a
maximum flow of 6 m3/h and a maximum outlet pressure of 1 bar.

Figure 1: Gas Absorption Column (Edibon M7, Spain).

42
.
Figure 2: Schematic diagram of Gas Absorption Column (Edibon M7,
Spain).

Specifications and useful data for calculations

• The column diameter is 75 mm, and its height is 1400 mm.
• Packing 8 mm glass Rasching rings

Procedure
E. Preparation of the Experiment:
(12) The column must be dried by passing the maximum air flow until all
evidence of moisture in the packing has disappeared.
(13) Connect the column top and bottom to the water manometer.

F. Starting of the Experiment:

a. Dry Column Experiment:
1. Ensure that the water pump is switched off.
2. Turn on the air compressor.

43
 3. Take manometer readings of pressure differential across the
column for a range of air flow rates.
b. Wet Column Experiment:
i. Switch on the water pump.
ii. Switch on the air compressor.
iii. Adjut the water flowrate at certain flow rate.
iv. Take manometer readings of pressure differential across the
column for a range of air flow rates.
v. Repeat the previous steps for a range of water flow rates.

44
 U7. Molecular Diffusion in Gases
1. Objectives:
1) To come up with experimental procedure to determine the diffusion
coefficient of a gas by evaporation from a liquid surface for acetone-air
system.
2) To compare the experimental value of the diffusion coefficient obtained with
theoretical predictions.

Note: Students will be provided with a standard experimental procedure

to use it to conduct their actual experiment after submitting the
Experimental Design Assignment.

2. Introduction:
Fick’s law of proportionality, DAB, is known as the diffusion coefficient. Diffusivity is
one of the important properties of fluids. Fluid flow and mass transfer operations
depend partially on this property and such data is always needed in plant design.
The diffusion coefficient depends on the pressure, the temperature and the
composition of the system. Specifically, the gas-phase diffusion coefficient is
• an inverse function of total system pressure
DAB α 1/P
• a 3/2 power-law function of the absolute temperature
DAB α T 3/2
For gaseous diffusion taking place, diffusion coefficients DAB and DBA are equal.
(This is not the case for liquid diffusion) [“Pseudo-Steady-State Diffusion” in
[Chapter 26] Welty textbook, page 409]

The Gaseous Diffusion Coefficients Apparatus allows students to measure the

diffusion coefficient to a reasonable degree of accuracy, by a well-established
technique. The practical exercise involved in this measurement allows students an
introduction to handling the basic equations of mass transfer.

45
 Figure 1 Image of the gaseous diffusion apparatus

Figure 2 Sketch of the gaseous diffusion apparatus

Modern versions of the kinetic theory have been attempted to account for forces
of attraction and repulsion between the molecules. Hirschfelder et al. (1949)
using Lennard-Jones potential to evaluate the influence of the molecular forces,

46
presented an equation for the diffusion coefficient for gas pairs of nonpolar, no
reacting molecules:
1/ 2
 1 1 
0.001858 T  3/ 2
+ 
D AB ,theo =  MA MB 
1
Pσ AB Ω D
2

where, T is the absolute temperature in K; MA and MB are the molecular weights A

and B, respectively; P is the absolute pressure in atmospheres; σ AB is the “collision
diameter”, a Lennard-Jones parameter, in Å; and Ω D is the collision integral for
molecular diffusion, a dimensionless function of temperature and of intermolecular
potential field for one molecule of A and one molecule of B [Welty textbook, page
409].

Ω D is collision integral, a function of κT / ε AB , where κ is the Boltzmann constant,

which is 1.38 × 10-16 ergs/K. [Refer to page 409, Welty]
ε AB is the energy of molecular interaction for the binary system A and B, a Lennard-
Jones parameter, in ergs. ε AB is estimated by the following equation:
ε ABε ε 
1/ 2

= A B  2
k  k k 
σ AB = 1 / 2(σ A + σ B ) 3

3. Apparatus
The equipment consists of acrylic assembly which is subdivided into two
compartments. One compartment (4) is constructed from clear acrylic and is used
as a constant temperature water bath. The other compartment (15) incorporates
an air pump and the necessary electrical controls for the equipment. The assembly
is mounted on adjustable feet (6). Water in the bath is heated by a cartridge
element (7) which is controlled by an adjustable on/off temperature controller (11)
connected to a PTC temperature sensor (3) mounted in the wall of the bath.
Temperature in the bath is also indicated on a glass thermometer (1) mounted in
a gland on top of the bath. Air is supplied to the capillary tube via a flexible tube
(17) connected to the air pump. The air pump is switched on by operating the right
hand mains switch (14). The height of the liquid in the capillary tube is monitored
using a travelling microscope (10) mounted on a removable support stand (9)
which incorporates a vernier height gauge (8). The water bath is fitted with a lever
operated cock (5) to facilitate drainage using a piece of flexible tubing.
The equipment is connected to the electrical supply using the integral cable (13).
An Earth Leakage Circuit Breaker (RCCB) is installed at the right-hand end of the
equipment to protect the user in the event of an electrical fault. The electrical
components are protected by a mains fuse mounted at the rear of the equipment.

47
Note: The water bath will be damaged if the water temperature exceeds 80°C.
Ensure that the temperature controller is not set above 60°C in use.

48
The equipment is designed for bench-mounting on a firm level surface. It is a self
contained unit and needs only a temporary supply hose to the water bath, for initial
filling.
4. Safety Aspects:
This equipment is designed for safe operation. However there can be potential
hazards arising from the following:
1. Injury through misuse
2. Injury from electric shock
3. Burns from components at high temperature
4. Risk of infection through lack of cleanliness

Accidents can be avoided if the equipment is regularly maintained and staff and
students are made aware of potential hazards. Students must be supervised by a
competent member of staff at all times when in the laboratory. No one should
operate the equipment alone, do not leave the equipment unattended.
However, to give increased operator protection, Armfield Ltd have incorporated an
Earth Leakage Circuit Breaker (ELCB, alternatively called a Residual Current
Circuit Breaker or RCCB) as an integral part of this equipment. If through misuse
or accident the equipment becomes electrically dangerous, an ELCB will switch off
the electrical supply and reduce the severity of any electric shock received by an
operator to a level which, under normal circumstances, will not cause injury to that
person.

5. References
1. Lab Manual – Course handout, Chemical Engineering Department, Qatar
University.
2. Welty, J. R., C. E. Wicks, R. E. Wilson, G. L. Rorrer, Fundamentals of
Momentum, Heat, and Mass Transfer, Chapters 24 and 26, 5th Edition, John
Wiley & Sons, Inc.

49
50