Lab 1: Batch Tray Dryer

1. Introduction
The drying or dehumidification of material is an important process in several
industries because it affects the quality and storability of the product which involves
the production and transportation costs. In the majority of drying processes, hot air is
used as a medium for the heat to transfer so that water can vaporize out of the material.

2. Objectives
1. To develop and conduct appropriate experimentation, analyze and interpret
data, and use engineering judgement to draw conclusion through their
knowledge of heat and mass transfers regarding the drying performance
with different operating condition of the dryer for a given material.
2. To select appropriate air velocity from the experiment to achieve the desire
moisture content in the sample at a specified drying time.
3. To evaluate the heat exchanger performance inside the dryer.

3. Theory
Dryer usually consists of 2 parts:
1. Hot air preparation zone: air is heated using steam, electricity or other fuel.
2. Drying zone: moisture containing material is placed and allowed to contact
with hot air in this zone.
Dryer can be categorized from their operating character as batch and
continuous processes. The section for appropriate drying process depends on nature
and amount of material as well as quality of the desired product, availability and etc.
Examples of dryer normally used in many industries are pneumatic dryer, tray dryer,
conveying dryer, drum dryer and spray dryer.

3.1 Drying phenomena

Drying is a process that heat and mass transfer phenomena occur
simultaneously. Heat is transferred from the initially higher temperature heated air to
the sample material by convection, resulted in an increase in material temperature.
Water inside the material is vaporized to the surrounding hot air by driving force from

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the difference between vapor pressure of water inside material and partial pressure of
water in the air. The relationship between moisture content and drying time (drying
curve) is shown in Fig. 1. The shape of the plot may be different depending on the
properties of the moist material and the operating conditions (air characteristics) such
as hot air velocity, temperature and humidity (relative humidity, dew point or wet bulb
temperature).

A
B
Moisture content, M

MB
C
MC

E
ME

Time, t
Fig. 1 Drying curve.

From the reduction of moisture content along the drying time as shown in Fig.
1, the drying rate (or the amount of water evaporated per time, R) is related to the slope
of the graph and can be calculated by

̅
dM
R = −ws (1)
dt

Where R = Drying rate (g-water/h)

Ws = Dry weight of material (g-dry solid)
 g − water 
M = Moisture content in the material (dry basis)  
 g − drysolid 
t = Time (h)

The plot of the drying rate versus moisture content and the drying rate versus
time are then shown in Fig. 2.

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 Drying rate, R
C B

A
D

ME Moisture content, M

(a)
Drying rate, R

B C

A
D

Time, t

(b)
Figs. 2 Drying rate curves versus (a) moisture content and (b) time.

From Fig. 2, the first stage of drying process starts at point A with certain
amount of moisture content in the material. The drying rate could be slightly increased
due to the higher temperature of air when compared to the material. After that, for
various materials which contain high moisture content, there will be a constant drying
rate period (BC) and then the drying rate will be decreased slowly. The drying
mechanism is different in each period and is described as follow. In the earlier period
of the drying process (AB), the drying rate may be either increased or decreased and
it could happen too fast to be able to observe from experiment. This is the period
where the material is adjusting into steady-state. The next period is the constant drying
period (BC). Some materials with low moisture content such as some grains may have
a very short BC period or have no BC period at all. Moreover, in this period, the
moisture content inside the material is still rather high and the material surface is still

1-3
saturated with water. The material temperature is around wet bulb temperature of hot
air. Water inside the material is transferred to the material surface by diffusion and
then evaporates to the surrounding hot air by convection. As long as the moisture
inside the material is still high, the rate of transfer of moisture inside the material will
be equal to the rate of evaporation from the surface. As a result, the drying rate will
be constant at the beginning of the drying process (BC). In this period, if the drying
temperature or the hot air velocity is increased, the drying rate will be increased too.
This is because an increasing of temperature and velocity enhance the heat transfer
and mass transfer coefficients.
dM
From Equation (1), it can be seen that if the drying rate (R) oris constant,
dt
dM
then R can be determined from the experiment or calculated from the slope ( ) of
dt
the drying curve. Upon an integration of Equation (1) from B (M B ) to C (M C ) , the
total time for constant drying period (tc) can be calculated from

tc=
( Ws )
(MC − MB ) (2)
RC

Where RC = The constant drying rate

The constant drying period is ended at point C where the moisture content at this point
is called critical moisture content.

The period for decreasing rate of drying is the CE line in Fig. 1. As the
moisture inside the sample starts to decrease, the diffusion of water from inside to the
sample surface will be slow down and cannot compete with the evaporation of water
at the surface which will result in the decreasing of drying rate. This CE period can
be divided into CD and DE periods as shown in Fig. 2. The rate of drying in this
period is diffusion controlled, therefore an increase in air velocity will not make any
difference. On the other hand, with increasing of hot air temperature, the diffusion
coefficient will be increased and results in some incremental drying rate. The
determination of drying rate for this period is simple if the decreasing of drying rate is
linear. However, other forms beside linear are usually found as well.

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3.2 Equilibrium moisture content
As the drying proceeds (under any constant air condition), moisture content
inside the sample will reach a constant value (M E ) where further drying will no longer
decreases the moisture content of the sample. This shows that the drying reaches
equilibrium and the moisture content at this point (E) is called equilibrium moisture
content, M E . Equilibrium moisture content is a material property and depends on the
drying conditions such as temperature and relative humidity. Equilibrium moisture
content may not be zero but, at this equilibrium, the drying rate may become zero
because there is no driving force for heat and mass transfer. The temperatures of air
and material are the same and the partial pressure of water vapor in the air equals to
that inside the material.

3.3 Overall heat transfer coefficient

In general, a batch tray dryer consists of 2 parts: hot air production unit and
drying unit. From the experiment, the following parameters will be involved in the
hot air production unit: overall heat transfer coefficient among steam, finned tube and
hot air (U), convective heat transfer coefficient between steam and inner tube surface
or inside fluid film coefficient (hi ), conductive heat transfer coefficient through the
tube wall and fin (k) and convective heat transfer coefficient between outer tube wall
including fin and hot air or outside fluid film coefficient (ho ). The relationships
among these parameters are written below.

d
1 1 do ln( o ) d 1
di
= + + ( o) ( ) (3)
U𝑐 ho 2k d ih i

Where Uc = Cleaned overall coefficient based on the outside area of the tube
(W/m2.K)
ho = Outside fluid film coefficient (W/m2.K)
hi = Inside fluid film coefficient (W/m2.K)
k = Thermal conductivity of the tube wall material (W/m.K)
di = Tube inside diameter (m)
do = Tube outside diameter (m)

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 It is assumed that the surface area of the inner tube wall and the surface area
of outer tube wall including fin are the same and equal to Aa. Since the tube and fin
are made from copper which has very high heat conductivity, the conductive heat
transfer resistance term (the middle term of Equation (3)) will approach zero and then
the steam temperature ( Ts ) is approximately the same as the outer tube wall

temperature. In general, the value of hi changes only slightly with pressure and
temperature of the saturated steam, therefore Equation (3) becomes

1 1
= c1 + (4)
U ho

The value of ho in the forced convection system depends on air velocity or

Reynolds number ( Re ) and Prandtl number ( Pr ). When the air velocity is varied,
Equation (4) can be rewritten as

1 1
= c1 + (5)
U c 2 vn
a

Where c1 ,c 2 = Constants
va = Air velocity
n = Constant

The actual overall heat transfer coefficient can be calculated from the experimental
results as:

Q = UactualAaTlm (6)

Where Q = Heat transfer rate (W)

Aa = Surface area of the tube wall and fin (m2)

Tlm = Log mean temperature difference between steam and air streams (K)

The value of Q in Equation (6) can be obtained from experimental results by

calculating the enthalpy change of steam or increasing in the sensible heat of air. The
value of Uactual can then be calculated. Noted that the Uactual includes the fouling effect
on heat transfer, therefore, if Uactual is used in Equation (5), the c1 and c2 obtained are
also including the fouling effect.

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4. Experimental
Tray dryer used in this experiment is consisted of:
1. Air feeder, using a blower with a damper to adjust the air flow rate.
2. Heat exchanger (hot air production) which contains vertical copper finned
tubes with total surface area of 1.8 m2. Fed air is heated by a saturated steam
flowing inside the copper finned tubes. The saturated steam pressure is
adjustable.
3. Drying unit consists of a tray rack hanged from the top of the dryer. Both
wet bulb and dry bulb thermometers are attached to measure the air
temperatures inlet and outlet of the dryer. The air velocity can be detected
using a hot-wire anemometer.

The batch tray unit in this laboratory is shown in Fig. 3, where the detailed
of air feeder, heat exchanger and the dryer compartment are shown in Figs.
4 (a) to (c), respectively.

V1

V2
V3

Figure 3. The batch tray dryer unit.

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 (a) (b) (c)
Fig. 4 The details of (a) air blower, (b) heat exchanger and (c) the dryer compartment.

4.1 Equipment Operation

1. Air is fed air directly across the copper finned tubes (crossflow exchanger)
by opening the blower. The air velocity can be adjusted using a damper.
2. The saturated steam is fed through the inside of the copper finned tubes by
opening the valve V1 slowly. The valve V2 and V3 must be checked that
they are on the opening position before opening the valve V1. The saturated
steam pressure can be finely adjusted by the pressure regulator (V3) and its
value is shown at the pressure gauge.
3. Wet sample laid on the tray is placed into the tray rack inside the dryer
chamber by opening the door of drying chamber in zone 3 of Fig. 1.
4. Weight of the sample is measured using a digital balance placed outside the
drying chamber. The sample tray must be taking out from the drying
chamber to measure its weight.
5. Condensate flow rate is measured from the condensate outlet stream. Wet
bulb and dry bulb temperatures both inlet and outlet are measured using
thermometer as shown in Fig.1. The air flowrate is measured at the air outlet
position using a hot wire anemometer.
5. When the experiment is finished, the valves V1 and V3 are turned off to
stop the steam flow. When the dryer is cooled down to near room
temperature, the blower is then switched off.

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4.3 Operation variables
1. Air velocity: adjusted by a damper from the lowest to the maximum level.
2. Steam pressure: 0.5 – 1.5 bar gauge.
3. Operation time: maximum 45 min/batch
4. Different samples
5. Moisture content: 20 – 25% wet basis for the given sample
5. Sample tray: 1 – 4 trays.

Precaution:
1. During the experiment, the tube used for the wet bulb temperature
measurement should be fully filled all the time.
2. The condensate flowrate measurement should be performed at least twice
with a minimum volume of 500 milliliter each.
3. The preparation time before the wet sample is placed into the drying
chamber and the amount of wet sample used should be similar for all runs.
4. The drying unit is hot, especially the steam pipe and the heat exchanger
tube, great care must be taken into consideration while running the
experiment and recording all the data.
5. The condensate should be removed from its reservoir before it is fully filled,
to avoid the overflow and the slippery of the wet floor.

4.3 Answer the question (in the Appendix section)

If a 50 kg/hr wet sample with the moisture content of 20% wt (wet basis) is
fed into the tray dryer and then left the dryer with the moisture content of 4% wt
(wet basis), calculate the flowrates of the water evaporated and the dried product
obtained.

Before performing the lab, students must be able to explain about the basic
principles of the vapor – liquid equilibrium, phase diagram, vapor pressure, relative
humidity and the enthalpy change calculation which are not included in the theory of
this lab.

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6. References
1. วิวฒั น์ ตัณฑะพานิชกุล, 2522, อุปกรณ์ อบแห้ งในอุตสาหกรรม, สมาคมส่ งเสริ ม
เทคโนโลยีไทย - ญี่ปุ่น.
2. Mc. Cabe, W.L., Smith, J.C. and Harriott, P., 1985, Unit Operations of
Chemical Engineering, Mc.Graw-Hill.
3. Heldman, D.R. and Singh, R.P., 1981, Food Process Engineering, AVI.
4. Kern, D. Q., 1984, Process Heat Transfer.

Updated
27 February 2022

1-10
 Lab 2: Flash Evaporator

1. Introduction
Flash or partial evaporation is the partial vaporization that occurs when a
saturated liquid stream undergoes a reduction in pressure. If the saturated liquid is a
single condensable liquid, a part of the liquid immediately flashes into vapor. This
type of flash evaporation is used in the concentration of foods or fruit juices to reduce
the decomposition of valued components by heat.

1.1 Construction of evaporator

The evaporator is generally composed of:
1. Heat Exchanger: for heating feed solution and then vaporizing the solvent,
2. Separator: for separation of vapor and concentrated solution, and
3. Condenser: to condense vaporized solvent.

1.2 Construction of Flash Evaporator in this experiment

1. Evaporating tube: Jacket type, made from stainless steel with a surface heat
transfer area of 0.25 m2. Inside the evaporating tube, there are 4 stirred blades in order
to spread the solution into a thin film around the inner tube surface which is being
heated by steam flowing in the jacket.
2. Condenser: Jacket type with surface heat transfer area of 0.30 m2 (216
mm1350 mm). The vapors inside are cooled and condensed by water flowing in the
jacket.
3. Vacuum pump for reducing the pressure in the unit
4. Reservoirs of concentrated solution and condensate.

2. Objectives

To evaluate the appropriate condition of this evaporator

3. Theory
The overall heat transfer coefficient of the evaporating tube (heat exchanger)
can be determined from the following relation:

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 𝑄 = 𝑈𝐴𝑠 𝐹𝛥𝑇𝑙𝑚 (2)

where U = Overall heat transfer coefficient (W/m2C)

As = Inside surface area of evaporating tube (m2)
F = Temperature correction factor
Tlm = Log mean temperature difference between heating medium (steam)
and boiling liquid (C)

The heat required to heat the feed solution and partial vaporize the solvent can
be calculated from energy balances as follow:

Q = L F C pF (Tb − TiF ) + V0  0 (1)

where LF = Mass flow rate of feed (kg/s)

CpF = Mean specific heat of feed stream (J/kgC)
Tb = Boiling point of liquid corresponding to operating pressure (C)
TiF = Temperature of feed stream inlet (C)
V0 = Mass flow rate of solvent vaporized in evaporator (kg/s)
0 = Latent heat of vaporization of solvent at operating pressure and
corresponding saturation temperature (J/kg)

4. Experimental
A Schematic diagram of the flash evaporator unit is shown in Fig. 1.

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 Condenser Evaporating tube
Steam
P-2

V-5

V-2 V-1 V-6

C-2 V-7
V-1 Leak valve
Reservoir 2
Reservoir 1
Concentrated
Condensate P-1
solution

V-4 V-3

Leak valve
Vacuum pump

Fig. 1 Schematic diagram of flash evaporator unit.

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 Fig 2 Flash evaporation unit

4.1 Equipment operation

1. Put the feed line into the feed tank
2. Flow water into the condenser and mechanical seal of the motor.
Warning: Do not switch on the stirred motor before feeding water into the
mechanical seal to prevent burning of the motor.

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 3. Close V-3, V-4, V-7 and leak valves to prevent outside air from flowing
into the evaporator. Then, switch on the vacuum pump and turn on the red
valve at the vacuum pump. Check the pressure in the evaporator and wait
until the pressure is close to the 0 bar.
4. Switch on stirred motor and adjust stirred speed. At the same time, feed
steam into the jacket of evaporating tube and adjusting steam pressure.
Simultaneously, feed the sugar solution into the evaporating tube by
opening the flow meter valve and adjusting the feed flow rate.
7. To terminate the experiment, turn off the stirrer, steam and feed. Close the
red valve at the vacuum pump and then switch off the vacuum pump. To
discharge the condensate and concentrated solution from the reservoir, the
leak valve must be opened.

4.2 Operation range

1. Stirred speed 100-700 rpm.
2. Steam pressure 0.5 – 1 bar gauge.
3. Feed flow rate 20 – 40 l/min.
4. Feed concentration 3-5 Brix.
5. Operation time 20 min.

4.3 Caution
1. Before switching on stirred, the stirred speed must be at 0 rpm.
2. When the stirrer is rotated, be sure that it has solution feeding into the
evaporating tube.
3. If the equipment is vibrating or the stirrer has high noise, decrease the stirred
speed.
4. After finishing the experiment, the water must be drained from the steam trap.

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 Steam trap

4.4 Cleaning procedures

4.4.1 Cleaning of the evaporating tube
1. Close the V-1 valve and turn on the vacuum pump.
2. Feed water into the evaporating tube.
3. Switch on the stirred motor.
4.4.2 Cleaning of the condenser
1. Use the same method as cleaning the evaporating tube but the water flow
must be high enough for flowing through the condenser.

Remarks
The students must explain the following question during the laboratory brief.
1. What is flash evaporation?
2. How to obtain flash evaporation?
3. How a decrease in pressure can affect the boiling point of the substance?
Why?
4. How the equipment used for the flash evaporator is different from the
normal evaporator?

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5. Simply sketch the flash evaporator and explain the process of flash
evaporation.
6. Draw the evaporating tube section and specify the flow streams and
direction. Also, explain the heat transfer and write the total equation of the
overall heat transfer coefficient.
7. Write the heat transfer rate of the heat exchanger and explain the meaning
each parameter.
8. Write the heat transfer equation for both the steam side and solution sides.
Also, explain the meaning of each parameter.

Updated
13 February 2022

2-7
 Lab 3: Multistage Continuous Distillation

1. Introduction
In chemical process industries, the production of any chemicals involves
several process operations, such as reaction, separation and utility sections. Basically,
the reaction section is considered to be the core of the process while the separation
section deals with the purification task to achieve the desired product quality. To
obtain the required product specification/purity, the operation of separation section is
therefore very important. At present, the major separation unit used in industries is
distillation column. Although it is an energy intensive unit, distillation is still very
popular since it can handle high separation capacities in a large-scale production plant.
Distillation column can be found in various configurations ranging from a very simple
column with only a single column shell to complex columns with several
interconnected column sections. It can also be operated in two modes, i.e. batch and
continuous. The application of batch distillation column can be found in small - scale
industries such as food and pharmaceuticals whereas the continuous distillation is
generally applied in large-scale industries such as refineries, or petrochemicals.
In this laboratory, the study is focused on the operation of a simple distillation
column in continuous mode. The students who have completed this laboratory test
will understand basic principles in distillation and know how to efficiently start-up
and operate a simple continuous distillation column in real industries.

2. Objective
Determine the suitable operating condition to get 95% ethanol and
column efficiency.
3. Theory
3.1 Brief theory
Distillation is one of the oldest and still most common methods for both the
purification and the identification of organic liquids. It is a physical process used to
separate chemicals from a mixture by the difference in how easily they vaporize. If
one compound is much more volatile than the other, the compounds can be separated
in one vaporization step. Such a step is called simple distillation and uses an apparatus
that consists of only a pot, a distilling head, a condenser and a receiver (see Figure 1).

3-1
When the boiling points of two compounds differ by less than 40ºC, they cannot be
separated by simple distillation. Fractional distillation, a process that is more efficient
than the simple distillations, must be used. A fractional distillation apparatus includes
a fractionating column placed between the pot and the distilling head (see Figure 2).
Typically, any one of a variety of materials, including glass beads and metal sponge,
fill the fractionating column. In large chemical plants, any industrial - scale column
may consist of several trays instead of packing materials to perform this fractionating
function. It can also be called a multistage distillation column.

Figure 1: Simple distillation [1]. Figure 2: Fractional distillation [1].

A simple distillation is often considered when:

a) The liquid is relatively pure to begin with (e.g., no more than 10% liquid
contaminants).
b) Essentially a pure material is separated from a non-volatile or from a solid
contaminant.
c) The liquid is contaminated by a liquid with a boiling point that differs by
at least 70°C.

Simple distillation involves a single equilibrium stage between the liquid and
vapor. This distillation is referred to as involving one theoretical plate.

3-2
 To understand the nature of simple distillation and fractional distillation, we
need to look at vapor/liquid diagrams for pairs of solvents. The graph in Figure 3
shows such a diagram for 2 solvents, A and B. A is the lower boiling substance. The
bottom of the graph shows the liquid state and the top of the graph shows the vapor
state. The area between the two curves shows what is happening in the distillation
column. If we start with a mixture of A and B that corresponds to the dashed white
line on the graph and the letter C1 (concentration 1), the mixture is vaporized (follow
the horizontal blue line until it reaches the vapor curve). This is concentration C2 in
the diagram. This process has improved the concentration of A, the lower boiling
component. The material is then condensed (follow the white vertical line down to
the liquid curve). If this was simple distillation, we could stop now. It can be seen
that the purification affected by the simple distillation of such a mixture of volatile
liquids is improved to only a small degree.

Figure 3: T-xy diagram showing a distillation path of a binary mixture [1].

However, in a fractional distillation, the distillation process continues. The
condensed material is vaporized again. Follow the blue horizontal line across from
the liquid curve at C2 to the vapor curve. There is another improvement in the
concentration of the lower boiling component A. The vapor is condensed again.
Follow the white vertical line down to the liquid curve. This number of times that the
process of vaporization and condensation occurs depends on the efficiency of the
distillation column. The more efficient the distillation column, the more times this
happens and the purer the final product will be.

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 The separation efficiencies of simple distillation and fractional distillation can
be compared by monitoring the change in the overhead temperature during the
progress of the distillation. From Figure 4, it can be seen that the overhead temperature
change is more rapid in case of a fractional distillation when compared to the curve
obtained during the course of a simple distillation. As a result, a higher distillate purity
of volatile component can be achieved with a fractional distillation.

Figure 4: Changes in overhead temperature during the course of distillation [2].

With azeotropes, the vapor-liquid curves are not ideal and have a point where the
vapor curve meets the liquid curve. This point is called an azeotropic point. In such case,
a nearly pure product could not be obtained even by means of a fractional distillation. The
T-xy curves of such system are shown in Figure 5.

Figure 5: T-xy diagram of a non-ideal binary mixture showing a minimum

azeotropic point [1].

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 For continuous multistage distillation as shown in Figure 6, these stages can
be stacked into column with multiple trays. The continuous separation of a binary
mixture into high purity product can be represented by a T-xy diagram (Figure 7) or
y-x diagram as commonly known as the McCabe-Thiele plot (Figure 8).

Vapour (V)

1 Vapour (V)

1
2
2
Feed (F) Feed (F)
3 3

4
4
5

Liquid (L)
Liquid (L)

Figure 6: Multistage distillation can be constructed as a single column with

multiple trays.

120
Constant Pressure
115

110
5
105
Higher purity product
Temperature (deg.C)

4
100
3
95 2

90 1

85
Higher purity product
80

75

70
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole fraction
Light Component

Figure 7: Multiple equilibrium stages of a continuous distillation on T-xy diagram.

3-5
 Distillate

0.9

0.8

Vapour Mole Fraction (Y)

0.7

0.6 Rectifying Section

0.5

0.4 Feed Location

0.3

0.2
Stripping Section
0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Liquid Mole Fraction (X)
Bottom Product

Figure 8: McCabe-Thiele plot of a continuous distillation on y-x diagram.

3.2 Required knowledge

Students should read/know:
• Theory behind McCabe-Thiele’s method and how to apply in the
analysis of the test results.
• How an operating line changes with reflux ratio.
• Ethanol-water VLE data at atmospheric pressure.

Basic readings:
• Geankoplis, C. J., 2003, Transport Processes and Separation
Process Principles, 4th Edition, Prentice Hall.
• King, C. J., 1971, Separation Processes, McGraw-Hill, USA.
• Lydersen, A. L., 1983, Mass Transfer in Engineering Practice,
JohnWiley & Sons, Ltd.
• McCabe, W. L. and J. C. Smith, 1976, Unit Operations of Chemical
Engineering, 3rd Edition, McGraw-Hill, USA.
• Perry, R. H. and D. W. Green, 2008, Perry’s Chemical Engineers’
Handbook, 8th Edition, McGraw-Hill, USA.
• Treybal, R. E., 1980, Mass-Transfer Operations, 3rd Edition,
McGraw-Hill, USA.

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4. Experimental Method
Figure 9 shows the schematic diagram of simple distillation. 200 l
ethanol solution is added into a TK 100 tank and Figure 10 shows a pilot ethanol-
water distillation column. Prior to start experiment, the ball valves at positions of
the column such as V-100, V-119 and V-131 are fully opened while the other
valves must be closed. Also, the ball valves at the cooling water are opened.
The fresh ethanol is fed through the column and E-101 reboiler by a P-100
pump. After the solution reached the desired level in the reboiler as indicated
by blue lighting turning on, the solution in the reboiler starts heating and the
temperature at this equipment is controlled at 100C. The vapor flows through
the column, and is condensed by E-100 condenser and collected at D-100 drum.
As the distilled ethanol accumulated at the drum is sufficiently enough for the
reflux. The P-101 reflux pump is turned on and the feed rate is controlled by
adjusting two ball valves (V-136 and V-138). The distilled sample collected in
the drum is withdraw to collect at TK-101 tank as the concentration at the drum
is above 90% by volume. In a distillation system, several kinds of vessels and
equipment are required to accomplish a steady-state operation.

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 Figure 9 Schematic diagram of simple continuous distillation

Figure 10: A pilot ethanol-water distillation column at ChE KMUTT.

4.1 Experimental Procedures

4.4.1 Column start-up
There are several ways to start-up a distillation column and operate at a steady-
state condition. Your task is to plan a start-up procedure in order to achieve the target
product purity within a short period of time. The ethanol purity of the top product
must be in a range of 90-95%vol at steady state while less than 3%vol ethanol is
required in the bottom product. The desired flow rate of a 10%vol ethanol feed must
be at least 50 liters/hr. Once reaching the steady-state, record the operating reflux rate
and the heat rate supplied to the reboiler.

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 • For safety reasons, the cooling water in the condenser should be kept
running along the entire experiment.
• In case of flooding conditions, switch off the heater immediately.
• In any emergency situation, turn off the heater but leave the cooling water
on.

4.4.2 Column shutdown

Heater must be turned off first while leaving cooling water to run until the
column is cooled down to around 50oC. After that, the cleaning-up procedure can be
carried out.

4.4.3 Cleaning up
• Check the bottom product purity in the bottom product tank. If the ethanol
purity is higher than 5%vol, leave the liquid in the tank to be used as dilution
water for other group. Otherwise, flush the liquid content down the drain
and clean up the tank.
• For any leftover liquid feed, recover it in the provided container and attach
a correct label of liquid purity. Then, clean up the feed tank.
• Recover the high purity distillate from the distillate product and the reflux
tank back into the original ethanol container, attach a correct label; then
keep it in a storage place.

5. References
[1] http://swc2.hccs.edu/pahlavan/2423L7.pdf
[2] http://courses.chem.psu.edu/chem36/Experiments/PDF's_for_techniques/Distilla
tion_&_BP.pdf
[3] http://classes.kvcc.edu/chm220/CHM220%20Distillation%20Lab.pdf
[4] http://www.nt.ntnu.no/users/preisig/Repository/TKP_4110_Felles_Lab/experim
ent%20descriptions/DistInstruct.pdf

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 Lab 4: Packed Tower

1. Introduction
Basically, the widely used separation methods in large-scale chemical
process industries are distillation or absorption/stripping. Both are the operations
occurring in a cylindrical tower with phase-contact apparatus inside. Either tray or
packing may be used to provide a contact between vapor and liquid flowing through
the tower. In a distillation, the separation occurs by applying heat to generate
heterogeneous phases (vapor from liquid) and enable the mass transfer of some
component between them, while the introduction of another immiscible fluid phase
(typically gas or liquid) to carry some components from the existing phase is the
main feature of the separation via absorption/stripping. The coexistence of vapor
and liquid phases in contact could lead to the mass transfer across the interface due
to the concentration driving force available between them. If the concentration
driving force is in the direction from gas to liquid, the mass transfer will occur from
the gas to liquid phase and this incidence is called absorption, such as the absorption
of acid gas by amine, or the VOC removal from air by absorption with water. On the
other hand, the mass transfer will occur from the liquid to gas phase if the
concentration driving force is in the opposite direction, and this process is known as
stripping, e.g., ammonia stripping by air.
In addition to the mass transfer phenomenon between the contacting vapor-
liquid phases, the fluid transport along the tower is also another significant incidence
affecting the stable operation. The tower hydraulics must then be investigated to
determine the appropriate operating range. Two main operating parameters
influencing both the tower hydraulics and the mass transfer characteristics are the
gas and liquid velocity in the tower. Setting these parameters inadequately will
result in operational instability such as tower flooding and high pressure drop.
In this laboratory, the study is focused on the operation of a packed tower
with dry bed and irrigated bed. The students who have completed this laboratory test
will understand basic principles in tower hydraulics and mass transfer characteristics
within the packed tower.

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2. Objectives
• To study the hydraulic characteristics of the packed tower.
• To determine the suitable operating conditions for ammonia stripping by air.

3. Theory
3.1 Brief theory
Hydraulics in packed tower
Typically, the packed tower is used to separate a desired component from one
phase by contacting with another immiscible phase. For the absorption, the liquid is
introduced as a carrier phase to scrub the required component from gas, e.g., the
hydrogen chloride removal in the chlorination process. For the stripping, the gas
phase is used to strip the light component from the impure liquid. During the
absorption/stripping operation, the flow of gas through the wetted packing will
exhibit a pressure drop across the packed bed. This could cost high electricity bill
for the gas driving equipment such as compressor or blower. Therefore, the energy
loss due to this pressure drop should be reduced to as low as possible. The adequate
operating flow conditions of both gas and liquid phases are thus very crucial for
successful and energy-efficient operation. In general, the pressure drop across any
packed section depends on the packing type, size as well as the types of material.
Nevertheless, for any existing tower with specified type of packing, the gas and
liquid flow conditions are the most important factors influencing the value of
pressure drop. There are many correlations or monograms for the prediction of
pressure drop of several types of packing. All of them are obtained empirically with
most data from the testing of air-water system. A simple form of correlation for the
prediction of pressure drop across the packing section is shown below [1]. It is used
for irrigated tower and can be applied to several types of random packing.

G2
P =   10L  (1)
g

When P = Pressure drop (in. H2O/ft packing)

g = Gas density (lb/ft3)
G = Gas mass velocity (lb/ft2 sec)

4-2
 L = Liquid mass velocity (lb/ft2 sec)
  = constant, given in the Table 1 for Raschig ring with various sizes

Table 1 The Constants in Equation (1).

Type of packing Nominal Size (in.)  

Raschig Rings 1/2 3.1 0.41
3/4 1.34 0.26
1 0.97 0.25
1½ 0.39 0.23
2 0.24 0.17

Generally, both gas and liquid will flow through the void in packed bed with
the gas phase occupying most of the void space. It is then considered as the
continuous phase while the liquid flowing down along the surface of the packing
could be considered as the dispersed phase. However, at the high gas flow
condition, the resistance to the liquid flow becomes so large that the accumulation of
liquid phase in the void space of packing can occur. Until reaching the flooding
point, the liquid finally fills in most of the void space and becomes the continuous
phase instead. At this point, the gas pressure drop will be very high and a large
amount of energy is necessary for the gas to flow pass both the void of packing and
the thick layer of flooding liquid. The gas flow is not uniform at the flooding point
and may result in the damage of packing if some are entrained from the tower at high
gas velocity. The loss of liquid may also occur in the form of the entrained liquid
droplets at the top of the tower at flooding point. The flooding location in the tower
depends on the flow of gas and liquid. At high gas flow, the flooding usually occurs
around the top of the tower, while the bottom flooding is found at high liquid flow.

Mass transfer in packed tower

The fundamentals of mass transfer between vapor-liquid interface in
absorption and stripping processes are similar except the direction of mass transfer.
Here, the mass transfer in stripping process will be studied. The stripping is the
mass transfer of solute which is typically light component or light gas from the
liquid to vapor phase by using the inert carrier gas.

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 For convenience in calculation and analysis of the stripping process, the
concentration driving force will be written in term of liquid-phase concentration as
follows:

x = x −x* (2)

The equation of mass transfer rate can be written as:

dN = A K L a (x − x *)dZ (3)

For dilute solution, Henry’s law could be applied.

p* = Hx* (4)

Dividing by total pressure on both sides yields:

p* Hx*
=
P P

p*
Where = y * , Equation (2) can now be written as:
P

y *P
x = x− (5)
H

For solutions not obeying the Henry’s law, the definition of equilibrium constant can
be applied.

y*
K = (6)
x*

For these solutions, Equation (2) can be written as:

y*
x = x− (7)
K

4-4
For solution at low concentration, the equilibrium line will be close to a straight line.
Additionally at low mass transfer rate comparing to the liquid flow, the operating
line will also be the straight line. Integration of Equation (3) will then be obtained.

N = A Z K L a x LM (8)

x1 − x 2
Where x LM =
x
ln 1
x 2

The mass transfer rate can be determined by:

N = L (x 1 − x 2 ) (9)

From these equations, the overall mass transfer coefficient can be determined from
the experiment. In this case the solution is dilute so the operating line and the
equilibrium line are straight. By equating Equations (8) and (9) we can obtain

Z = N OL H OL (10)
( x1 − x 2 )
where N OL =
x LM

L/ A
H OL =
KLa

The overall height of a transfer unit ( H OL ) can be easily determined from the
experiment.
3.2 Required knowledge
Students should read/know:
• Fundamentals of mass transfer between vapor-liquid interface in
stripping process and how to apply them in the analysis of the test
results.
• Equilibrium constants of ammonia solution data at atmospheric
pressure.
• Analysis of ammonia concentration in solution.
Basic readings:

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 • Geankoplis, C. J., 2003, Transport Processes and Separation
Process Principles, 4th Edition, Prentice Hall.
• King, C. J., 1971, Separation Processes, McGraw-Hill, USA.
• Lydersen, A. L., 1983, Mass Transfer in Engineering Practice,
JohnWiley & Sons, Ltd.
• McCabe, W. L. and J. C. Smith, 1976, Unit Operations of Chemical
Engineering, 3rd Edition, McGraw-Hill, USA.
• Perry, R. H. and D. W. Green, 2008, Perry’s Chemical Engineers’
Handbook, 8th Edition, McGraw-Hill, USA.
• Treybal, R. E., 1980, Mass-Transfer Operations, 3rd Edition,
McGraw-Hill, USA.

4. Experimental Method
4.1 Experimental Procedures
Figure 1 shows the schematic diagram of a packed tower.

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 Figure 1. A packed tower at ChE KMUTT.

4.4.1 Packed tower start-up

To start up the dry bed, follow the procedure below.
• Switch on the air blower while adjusting the air inlet valve at maximum
opening.
• Adjust the gas flow to the target value. Leave the system to reach a steady
state, then record the operating parameters required.
To start up the irrigated bed, follow the procedure below.
• Switch on the pump and adjust the water flow to the target value.
• Switch on the air blower and adjust the gas flow to the target value.
• Leave the system to reach a steady state, then record the operating
parameters required.
To start up the stripping mode, follow the procedure below.

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 • Prepare the ammonia solution at approx. 0.1 wt % concentration for 300
L. Then adjust the solution pH to the optimum value using NaOH
solution.
• Switch on the pump to feed the ammonia solution into the tower and
switch on the air blower to feed the air flow into the tower.
• Record the operating parameters required.
Limitation of equipment: the air blower must be operated lower than 3,000 rpm and
the water (solution) flow must not exceed 10 LPM.
4.4.2 Cleaning up
• Flush the liquid down the drain and clean up the tower and feed tank.

4.4.3 Packed tower shutdown

• After the cleaning-up process is done, all switches must be off.
4.2 Safety precautions

Care should be taken when operate at the irrigated condition. From Fig. 2,
showing the detail at the bottom sump of the tower, the liquid level in the sump
should be maintained at normal level in order to prevent the air escaping from the
bottom. However, the maximum liquid level should not be exceeded otherwise the
liquid will flow back into the blower line thereby causing great damage to the
blower. Should this backflow of liquid ever happen, the blower must be switched
off immediately while draining the excess liquid from the system as fast as possible.

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 Air Inlet

Max. Liq. Level

Normal Level

Water Outlet

Figure 2. The detail of bottom sump of the packed tower.

• Chemicals used in this experiment may irritate the skin, eyes, and
respiratory system, hence minimize your contact with the chemicals and
their vapors.
• Smoking is absolutely prohibited inside the workshop.
• Wear goggles when charging, discharging, or taking samples of the liquid
from the process.
• Chemical resistance gloves must be worn when taking samples.
• Wash your hands thoroughly with soap or detergent before leaving the
workshop.

Dress codes:
• Wear workshop uniform at all times while working in the workshop.
• Wear trousers which entirely cover your legs. No shorts or skirts
allowed!
• Your hair must be tied-up.
• Wear covered shoes or boots! (no sandals, no high-heeled fashion shoes)

Safety Aids:

4-9
 • Locate the fire exit in the workshop.
• Prepare the fire extinguisher close to your working space and ensure that
you know how to use it correctly.
• Locate the fire aid box in case of emergency.
• Locate the eye wash and wash basin near your working place.

In case of fire, identify the fire area and then move away into safe place.
Evaluate the situation, if you can handle the fire, use the provided fire extinguisher
otherwise call for help.

6. Reference
1. Leva, M., 1951, Tower packings and packed tower design, The united
states stoneware co., USA, pp.33.

Updated
1 st August 2022

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 Lab 5: Process Control

1. Introduction
In chemical process industries, the production of any chemicals must be carried
out efficiently in the rapidly changing world. Therefore, the efficient utilization of raw
material and energy in the process become increasingly significant. The other issues
which also force the process performance requirement to a higher level of standard
are, for example, stronger competition, tougher environmental and safety regulations.
To satisfy all these aspects, process control has become a very important issue in
process operation. In addition, modern chemical plants become more complex and
difficult to control since there are several control loops interacting with one another in
the plant. Typical single - loop analog controllers may not be able to efficiently control
the overall process. Hence, the application of computer - based control system
becomes inevitable to achieve the above goals. It is therefore very important for
chemical engineers to have a good understanding of various aspects of process control
in terms of both theory and practice.
In this laboratory, the study is focused on a system with simple process control.
The students who have completed this laboratory test will understand basic principles
of typical feedback control and know how to efficiently create a simple process model
from experiment, and tune the controller to obtain the optimum control performance.

2. Objectives

1. To determine a PID controller setting by frequency response analysis.

2. To determine a stability by Bode stability criterion.

3. Theory
3.1 First Order Time Lags
Ideally, if the engineering value of a process variable changes, we would like
the sensing element to react to this change immediately and synchronously. However,
this is never the case. There will always be a lag in the sensing device. Similarly, we
would like to see the movement of a valve actuator to exactly and immediately follow
the output of the controller. Although there are devices that respond quickly to an

5-1
external influence, no device responds instantaneously. There is always some form of
lag. This lag is referred to as a time lag.
Consider the following scenario. An RTD type of temperature sensor is
stabilized at room temperature, and then suddenly immersed in a beaker of water at a
temperature of 20 oF above the ambient air temperature. This would constitute a step
change in input signal (temperature) to the RTD. Ideally, the output of the RTD would
follow the input signal. However, the RTD has mass. As such, it takes time for the
temperature of this mass to rise such that the resistance of the device changes. As
shown in the figure below, the output signal will not rise immediately. First, a certain
amount of time will pass before anything happens. This would be a dead time. Once
the dead time has passed, the output of the RTD will increase slowly and at a variable
rate. The results are shown as a response curve referred to a first order lag plus dead
time (FOLPDT). The terminology refers to the type of mathematical equation, a first
order differential equation, used to describe this response.
The shape of this curve is described by a time constant. The time constant of
a first order response is equal to the amount of time it takes to achieve 63.2% of the
total output. The time constant can be determined graphically as indicated in the
Figure 2. Assume the step function that generated this response occurred at time t=0.
The procedure for finding the time constant is as follows.

Figure 1. Graphic determination of time constant for first order lag.

• Draw a horizontal baseline tangent to the final value of the response curve
(100%).

5-2
 • Dead time occurs from time t=0 to the point of initial response (5s).
• Draw a tangent line to the steepest part of the curve until it intersects the upper
baseline. The steepest part of a true first order response always occurs at the
end of the dead time.
• From the intersection of the tangent line to the upper baseline, draw a vertical
line to the time axis. The difference between this time and the end of the dead
time represents the time constant of this first order response. In Figure 2, the
time constant is 10 seconds. Also note the vertical crosses the response curve
at a point equal to 63.2% of the total change in output.

3.2 Feedback control

Figure 2. Block diagram of a feedback control system.

Feedback control scheme is probably the most widely used control scheme in
industries. Dated back from the Greek era when this concept was used to control water
level in the tank [3], it is now applied in many kinds of application such as flow,
pressure, temperature, or composition control. The basic components in a feedback
control loop are shown in Figure 2. As the value of the controlled variable changes
due to any disturbances entering the process, it’s measured by a sensor that sends an
appropriate process signal back to the controller. In other words, the controller
measures the result of the change, and then takes some actions to rectify the change
by sending output control signal to adjust the control device in the process.
The standard feedback control algorithm is Proportional-Integral-Derivative
(PID) control. This control algorithm consists of three control modes. Mostly, only
some control mode or a combination of them may be applied. Examples of the control
modes used in industries are Proportional-only (P), Proportional-Integral (PI) and

5-3
Proportional-Integral-Derivative (PID). The equation used to calculate controller
output is shown below.

1 𝑡 𝑑(𝑒𝑟𝑟𝑜𝑟)
𝐶𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑟 𝑜𝑢𝑡𝑝𝑢𝑡 = 𝑏𝑖𝑎𝑠 + 𝐾𝑐 [(𝑒𝑟𝑟𝑜𝑟) + ∫ (𝑒𝑟𝑟𝑜𝑟) 𝑑𝑡 + 𝜏𝐷 ]
𝜏𝐼 0 𝑑𝑡

Change in controller output signal depends on three terms in bracket on the

right-hand side which represent Proportional, Integral and derivative effects,
respectively. There are three controller parameters, i.e. Controller gain (Kc), Integral
time (τI) and Derivative time (τD). Controller gain is different from process gain as
shown in the equations below according to the point references in Figure 2.

𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑝𝑟𝑜𝑐𝑒𝑠𝑠 𝑜𝑢𝑡𝑝𝑢𝑡 𝑠𝑖𝑔𝑛𝑎𝑙 𝑎𝑡 𝑝𝑜𝑖𝑛𝑡 2

𝑃𝑟𝑜𝑐𝑒𝑠𝑠 𝐺𝑎𝑖𝑛 = 𝐾𝑝 =
𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑐𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑟 𝑠𝑖𝑔𝑛𝑎𝑙 𝑡𝑜 𝑝𝑟𝑜𝑐𝑒𝑠𝑠 𝑎𝑡 𝑝𝑜𝑖𝑛𝑡 1

𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑐𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑟 𝑜𝑢𝑡𝑝𝑢𝑡 𝑠𝑖𝑔𝑛𝑎𝑙 𝑎𝑡 𝑝𝑜𝑖𝑛𝑡 1

𝐶𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑟 𝐺𝑎𝑖𝑛 = 𝐾𝑐 =
𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑝𝑟𝑜𝑐𝑒𝑠𝑠 𝑠𝑖𝑔𝑛𝑎𝑙 𝑡𝑜 𝑐𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑟 𝑎𝑡 𝑝𝑜𝑖𝑛𝑡 2

The students are encouraged to study in more detail of the properties of each control
mode from Ref. [3].

3.3 Controller tuning (Excerpt from [2])

Once a process and associated control components are installed, the control
loop must be calibrated to perform in the manner intended by the designer. This is
referred to as control loop tuning.
Before you set out to tune a control loop, you need to ensure the followings.
• All sensor/transmitters must be calibrated to manufacturer’s specifications
• The end device must be properly sized for the process. This implies all parts
of the system must be linearized to minimize variation in process gain over the
normal operating range of the process.
• Valves and dampers must be properly serviced to minimize sticking friction
• All linkages must be properly configured to eliminate performance errors.

If you do not take the time to ensure all elements of the process and control
loop are properly configured, the time taken to tune the loop will likely be wasted.
Not only are there different mathematical implementations of the ideal controller

5-4
equation, but also, each process being controlled may have a different mathematical
model. Even if the end result of two different processes is similar, there is likely to be
different values of dead time and time delay. These similar process differences may
require different tuning parameters, even if identical controllers are used, so as to allow
the control loop to respond as desired.
When one considers the number of controller structures available, coupled
with the large number of process models in existence, one can surmise that different
tuning rules may be necessary for each unique application. In fact, dozens of tuning
rules have evolved over the years to handle such combinations of different controllers
and different processes. Some of these tuning rules are quite formal and highly
mathematical in nature. Others are strictly trial-and-error and should generally be
avoided. Between these extremes are semi-formal methods that combine a structured
trial-and-error approach with minimal mathematic calculation. These semi-formal
methods tend to work well in the field. They are a good compromise between the more
sophisticated mathematical methods and the time required to perform the less accurate
trial-and-error methods.
The controller tuning methods may be classified into 2 major categories, i.e.
model-based tuning and on-line tuning methods [3]. The model-based tuning can be
carried out during the process design stage, if a reasonably accurate dynamic model
of the process is available. This technique can also be used to design feedforward
controllers and advanced control systems. However, if the process models used to
calculate the preliminary controller settings are not exact, the on-line tuning methods
based on simple experimental tests are often required.
There are several on-line tuning methods available in practice, e.g. trial-and-
error method, continuous cycling method and process reaction method. Although
being the simplest one, the trial-and-error method is not very popular due to its time-
consuming nature. Moreover, the optimum loop response from the tuning parameters
cannot be guaranteed. The other two methods can still find their applications in
process industries, hence will be described here in more detail.
One should also realize each tuning method will likely produce a different set
of tuning parameters. Even different persons using the same tuning method on the
same loop may arrive at different parameters. This is simply because two-mode and
three-mode controllers have numerous response curves occurring at different

5-5
oscillatory frequencies. What we wish to do is determine a set of tuning parameters
that is optimal for the process at hand.

3.3.1 Process reaction methods

Process reaction methods of loop tuning are accomplished with an open loop.
In other words, the feedback portion of the loop is broken. When a step disturbance
is injected to the system, the system will respond in accordance with the time elements
associated with the loop and reach a new point of equilibrium. An analysis of this
response allows one to determine the appropriate controller tuning parameters to
achieve quarter amplitude damping. The following steps describe the data collection
phase of the open loop analysis.
• Place the controller in manual mode. Make sure the process is lined out. Make
a step change in the controller output. The step change should be as small as
possible, but should not exceed a 10% change. This change will force the
process to change in a fashion similar to Figure 3.
• Calculate a process gain, a process dead time, and a process time lag as
indicated in Figure 3. Make sure you draw the tangent line to the steepest part
of the reaction curve. Use the relations in Table 1 to determine the appropriate
controller tuning parameters.
• Enter the tuning parameters, place the controller back in ‘Auto’, and perform
a closed loop test. The test should result in quarter-wave damping.
• Tweak the settings as necessary.

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 Figure 3. Analysis of an open loop response.

Table 1. Ziegler-Nichols tuning parameters for quarter-amplitude damping using the

process reaction method.

Control Mode Kc τI τD
P 𝜏 --- ---
𝑇𝐷 𝐾𝑝
PI 0.9𝜏 3.33TD ---
𝑇𝐷 𝐾𝑝
PID 1.2𝜏 2TD 0.5TD
𝑇𝐷 𝐾𝑝

4. Experiments
4.1 Temperature - control test rig
The process flow diagram (PFD) of the test system to be controlled is shown
in Figure 4. The main pieces of equipment are the hot-water tank and the plate-and-
frame heat exchanger. Water in the hot-water tank will be heated by steam through a
steam coil. The stirrer inside is used to ensure a well-mixed condition in the tank. The
function of this tank is somewhat similar to hot utility in industries. The hot water
produced will be used to supply heat to the process through process exchangers. In

5-7
this case, a plate-and-frame heat exchanger represents a process exchanger using cold
water as a heat-required process stream. The heat transfer in this exchanger is counter-
current flow with hot water flowing downward while cold water flowing upward.
After supplying heat to the cold water, the hot water will be cooled down,
therefore returned to the hot-water tank again. To maintain constant temperature in
the tank at a specified set point, steam will be continuously injected into the coil. In
order to accommodate any disturbances such as changes in steam pressure, heat load
in the process exchanger, the steam flow must be adjusted automatically. A feedback
control loop is therefore needed. In this case, the temperature value in the tank will
be measured by a temperature sensor and transmitter (TT). The temperature signal
will be sent further to the temperature controller (TIC) to evaluate the action to be
taken. Then the output signal will be sent from TIC to the steam control valve to adjust
steam flow in the direction which can bring the system back to steady-state at the same
set point again.

Figure 4. PFD of the temperature-control test rig at ChE KMUTT.

The control system in this test rig is a small-scale SCADA system. It consists
of a touch screen control panel (IMARI) as an HMI, and several PLC units (Siemens)
acted as signal transmitters and controllers. The functions of the touch screen control
panel are plentiful such as the followings:
• To monitor process variables in various forms such as field-value display on
process flow diagram, dynamic profiles or data tables.
• To store on-line values in the built-in data-logger and write data to file for
future analysis.

5-8
 • To supervise the local PLCs according to operator requirement, such as
adjusting set point value or switch operation between automatic and manual
modes.
• To control on-off switch of some pieces of equipment such as pump, stirrer, or
motorized control valve.

The key panel screen is the P&I Diagram as shown in Figure 5. The simple
P&I diagram of this process is displayed together with several monitoring variables,
function and control buttons. The name and function of each part are described
according to the numbers in the figure as follows:
1. Screen buttons: They are used to switch to the required screen such as P&I
Diagram or the dynamic profile of any particular variable.
2. Save log data: It is a function button used to save all logged data stored in the
data-logger and write them into a text file (.csv format). The written data file
will be stored in the internal flash disk (C:\).

Figure 5: P&ID screen on the touch screen control panel of the test rig.

3. Copy file: This button is a function button used to copy a data file from the
internal flash disk to the user’s USB flash memory (E:\) via the USB port
provided in front of the control box.

5-9
4. Clear data: This button is used to clear all data stored in the data-logger. The
data files stored in the flash disk (C:\) will not be affected. This button is useful
when the user wants to clear all undesired data in the data-logger prior to any
new test-run.
5. Exit to panel setup: This button is used to return to the main panel setup screen.
On that screen, user can set the system date and time, and also manage the file
and data. To come back to the P&I Diagram, user can press “Run” button on
the panel setup screen.
6. Stirrer control switches: These buttons are used to switch on or off the stirrer
motor.
7. Stirrer speed: This field displays the value of stirrer speed in RPM.
8. Stirrer speed control switches: These buttons are used to adjust the stirrer speed
via the frequency adjustment through an inverter.
9. Valve control switches: These buttons are used to switch on or off the
motorized control valve.
10. Pump control switches: These buttons are used to switch on or off the hot-
water pump.
11. Auto/Manual control switch: This button is used to switch between automatic
and manual control modes.
12. PID setting on/off: This button is used to switch on or off the setting of PID
parameter values
13. P setting and reading: The reading field shows the read proportional gain value
while user can set a new value in the setting field via a numeric keypad. The
value of proportional gain is dimensionless.
14. I setting and reading: The reading field shows the read integral time value
while user can set a new value in the setting field via a numeric keypad. The
value of integral time is in minute.
15. D setting and reading: The reading field shows the read derivative time value
while user can set a new value in the setting field via a numeric keypad. The
value of derivative time is also in minute.
16. Set point display: This field is used to set a new set point of the tank
temperature via a numeric keypad.
17. Valve opening: The reading field shows the read valve opening fraction while
user can set a new value in the setting field via a numeric keypad. The value of

5-10
 valve opening fraction is in range of 0-1 (0-100%). The user can only set this
value in manual mode.

The locations of temperature measurements (TI101-105) in this system are also

shown. TI101 to TI104 are the temperature measurements around the plate-and-frame
heat exchanger while TI105 is the measurement in the hot-water tank. The notations
are as follows:
TI101: Hot water inlet temperature.
TI102: Hot water outlet temperature.
TI103: Cold water inlet temperature.
TI104: Cold water outlet temperature.
TI105: Tank temperature.

4.2 Check lists of things you’ll need

• A computer notebook.
• Pen and paper.
• Process control textbook.
• A USB Flash disk (Cleaned).

4.3 Experimental Procedures

4.3.1 Equipment operation

• The HMI is a touch-screen panel. Please be very gentle when pressing any
buttons and handle the equipment with care.
• To prevent any difficulties involving data storage and transfer, all previously
recorded data and stored files should be cleared before starting your
experiment. To do this, click “Format Disk C” to clear all data files in drive
C:/. The user needs to enter password “000000000” to perform this operation.
Then, click “Clear Recorded Data” to clear all data stored in the data logger.
• Press “Run” button to start recording the data and operating the system.
• In manual mode, bring the system to the first steady state by setting the control
valve at a certain opening % (5-10% should be adequate).

5-11
 • Before starting an open-loop tuning, you can press “Clear Data” button (No.4
in Figure 5) to clear all unused data since starting the system. Be very careful
when to use this function button. Do not use it during an experimental run.

4.3.2 Data recording

• The process data recorded in the data-logger can be written into a text file (.csv
format) which can be opened in Microsoft EXCEL. An example of data table
format is shown below.

Date Time TI101 TI102 TI103 TI104 TI105 Speed % Valve

(oC) (oC) (oC) (oC) (oC) (RPM) Opening
14/8/2014 11:35:33 34.7 32 29.6 32.8 35.1 86 10
14/8/2014 11:35:35 34.7 32 29.6 32.8 35.1 86 10
14/8/2014 11:35:37 34.7 32 29.6 32.8 35.1 86 10
14/8/2014 11:35:39 34.7 32 29.6 32.8 35.1 86 10
14/8/2014 11:35:41 34.7 32 29.6 32.8 35.1 86 10

• To save logged data to file and transfer the saved file to an external USB flash
drive, one should carefully follow these steps.
• On the P&ID screen, press “Save Log Data” button (No.2 in Figure 5). All
logged data will be saved into a text file (.csv format).
• Insert a USB flash drive into the USB slot in front of the control box, then
wait for the pop-up acknowledge screen. If this screen does not appear,
your USB flash drive may not be recognized, please use a new one.
• Press “Copy File” button (No.3 in Figure 5) to transfer your saved file
from C:/ to your flash drive (E:/). You have to select the file required to
be copied (“csv_XXX_XXX.csv”), and also specify the name of the file
to be written on your USB drive.
• In case that you have accidentally lost your data file, you can still use the
backup data file saved automatically every 30 minutes. The auto-backup
file will be named in this format “TEST_XXX_XXX.csv”.

4.3.3 Safety precautions

• Be very careful not to touch any live wires or connecting terminals.
• The stirrer speed should be less than 100 RPM. During stirrer operation, do
not leave the tank lid open.

5-12
5. References
[1] Wells, C.J., Industrial Networks - Supervisory Control and Data Acquisition
(SCADA), TechnologyUK, [Online], Available:
http://www.technologyuk.net/telecommunications/industrial_networks/scada.sht
ml [August 20, 2014].
[2] Marcks, R., HVA 240 PRINCIPLES OF PROCESS CONTROL, [Online],
Available: http://h240.marcks.cc/downloads.shtml [August 20, 2014].
[3] Seborg, D.E., Edgar, T.F., Mellichamp, D.A., and Doyle, F.J., 2011, Process
Dynamics and Control, 3rd ed., International Student Version, John Wiley &
Sons.

5-13
 Lab 6: Fluidization

1. Introductions
Fluidization is commonly defined as "the operation by which the fine solids
are transformed into a fluid-like state through contact with a gas or liquid" [1]. In
fluid beds, granules of a solid material are held in suspension by a fluid flowing
through the bed. The solid material thus takes on the character of a fluid. This
applies both to the fluid mechanic and thermodynamic properties of the material.
Fluid beds are in use in a wide range of applications in engineering, e.g. tempering
baths with even temperature distribution, powder coating plant, drying plant, or
furnace. The isothermal conditions found in fluid beds make them ideal for many
catalytic reactions, since yield and selectivity of the catalyst depend to a large extent
on both temperature level and uniformity. Thus an important application of fluidized
bed heat transfer is in the design of commercial catalytic reactors. Another important
industrial application of the fluidized bed heat transfer is the fluidized bed drying.
This is because of its high capacity of mass, momentum and heat transfer.

Due to all afore mentioned reasons and advantages of fluidized bed, this
experiment was designed to study the heat transfer principle and the factors affecting
a heat transfer in a fluidized bed.

2. Objectives
1. To understand the characteristic of a fluidized bed.
2. Proposed objective. (by student)

3. Theory
The term fluid bed describes a finely granulated layer of solid material
(mass) that is loosened by fluid flowing through it to such an extent that the particles
of solid material are free to move to a certain degree. The layer of solid material
takes on properties similar to those of a fluid. The operation by which solid particles
are transformed into a fluid-like state through suspension in a gas or liquid is called
fluidization.

6-1
3.1 Interaction between solid and fluid
From Fig. 1, a solid particle with a diameter “d” and a mass “m” places in an
area that a fluid is passing upward through this particle with a velocity “v”. There are
three forces acting upon this particle, namely gravity force (mg), buoyancy force
(Fb) and drag force (Fd). The drag force is the force occurring by flowing a fluid
around the solid particle and it is proportional to the fluid velocity (v). Thus at a
certain fluid velocity, those three forces become balance and the solid particle will
move in the flowing direction of the fluid.

Fig. 1 Interaction of solid and fluid.

3.2 Characteristic of particle bed

When a fluid is passed upward through a bed of fine particles at a low flow
rate, the fluid merely percolates through the void spaces between stationary particles.
This is called a “fixed bed”. As the fluid velocity increases to a certain value, a point
is reached where all the particles start moving and are suspended. The bed is
considered to be just fluidized and is referred to as an incipiently fluidized bed or a
bed at minimum fluidization. Further increase in flow rate above minimum
fluidization usually results in a smooth, progressive expansion of the bed and the
solids are carried out of the bed with the gas. The bed is in the stage of
transportation. The characteristic of each stage of bed is displayed in Fig. 2.

6-2
 Fig. 2 Characteristic of the bed particles.

3.3 Physical characteristic of fluidized bed

While the bed particles start to suspend, the weight of particle and the drag
force are equal. The pressure drop across the bed is the highest at this initial stage.
The fluid velocity at this point is called “minimum fluidization velocity”. The
relationship between pressure drop across the bed with fluid velocity is depicted in
Fig. 3.

Fig. 3 Relationship between pressure drop across the bed with fluid velocity.

6-3
3.4. Heat transfer
Heat transfer mechanism in a fluidized bed composes of unsteady state heat
conduction of bed particles, heat convection of fluid in the form of bubbles, and
radiation of both phases. The relationship between heat transfer coefficient and fluid
velocity is displayed in Fig. 4.

Fig. 4 Relationship between heat transfer coefficient and fluid velocity.

At low fluid velocity, bed particles are in the stage of a fixed bed. The heat
transfer coefficient is low. Heat transfer depends on the heat convection of the fluid
passing through the void in the bed and the heat conduction of the solid in contact
with the heat transfer surface. In a fluidized stage, heat transfer between bed
particles and heat transfer surface turn to be more significant. Higher fluid velocity
causes the higher in heat convection of fluid and results in an increase in the overall
heat transfer. In solid removal condition, the amount of solid inside the bed
decreases and the heat conduction is lower. Consequently, the overall heat transfer
is lower.

4. Experimental
A lab-scale gas-solid fluidized bed set used in this experiment is shown in
Fig. 5 and the variables to be recorded are displayed in Fig. 5 and 6.

6-4
4.1 Chemicals and equipment available in the lab
1. Aluminum oxide ZWKS54 and ZWKS100 as bed particles
2. Digital balance
3. Ruler
4. Beaker
5. Lab-scale Gas-Solid fluidized bed set

6-5
Fig. 5 Lab-scale Gas-Solid fluidized bed set.

Fig. 6 The variables to be recorded.

6-6
4.2 Procedures (Design of Experiment)
Explain your designed procedures step by step and in a full detail according
to the given objective and the proposed objective.
4.3 Care and maintenances
1. Use the variable-area flow meter to read the air flow rate if the air flow
rate is in the range of 10-124 L/min. If the flow rate is higher than 124
L/min, read the air flow rate from the orifice, in which the value is
displayed on the panel of apparatus.
2. Control the surface temperature of heater not to exceed 180ºC by adjusting
the electrical power supply.
3. Carefully adjust the heater load and pressure measuring sensor.
4. Carefully assemble and disassemble the glass cylinder while changing
particle.
5. “Do not discharge the particle”, the particle used must be stored
properly after the experiment.
6. Do not mix the bed of different particles -size together

5. Data Analysis and Discussion

Describe the obtained results with clear and thorough interpretation. The data
maybe presented in tabular or graphical form and describe calculation methods.
Anticipate results from theory. Estimate uncertainties in results and state any
adjustments or corrections to the procedures. If there is any resource being referred,
make certain that you cite all references correctly.

6. References
1. Kunii, D. and Levenspiel, O., 1991, Fluidization Engineering, 2nd
edition, Butterworth-Heinimann, Boston.
2. Botteriall, J.S.M., 1975, Fluid-Bed Heat Transfer, 1st edition, Academic
Press.
3. Pell, M., 1990, Gas Fluidization, 1st edition, Elsevier Science Publishers.
4. Basu, P. and Fraser, S.A., 1986, Circulating Fluidized bed Boiler design
and operate, Butterworth-Heinimann, Boston.

6-7
Appendix
A. Technical Data
Dimensions
LxBxH 900 x 455 x 850 mm
Weight 65 kg

Supplies
Electrical 230 V, 50 Hz, 16 A

Compressed Air
Connection Quick Action Coupling NW7.2
Requirement 300 (Maximum) L/hr
Pressure 2 (minimum) bar

Process Container
Volume 2.15 L
Cross-Section 95 cm2
Material Glass
Capacity 1 (approximate) litre

Safety Devices
Safety Valve: 0.5 bar
Heater Cut-Out: 200 C
Heater
Heater Power, Adjustable: 0-140 W
Surface Area: 13.35 cm2

Measured Parameter
Temperature
Air Inlet
PTC Sensor with Transmitter
Heater Surface, Fluid bed Temperature
Measuring Range : 0-100 C
Thermocouple K with Transmitter
Measuring Range : 0-400 C
Flow Rate
Variable-Area Flowmeter: 10-124 L/min
Orifice with Root Deriving Differential
Pressure Sensor: 50-300 L/min
Pressure
Electronic Pressure Sensor
Measuring Range : 0-25 mbar
Spring Tube Manometer: 0-1.6 Bar
Displays for Electronic Measurement
LCD Displays, 3 1/2 Digit
Background illumination
Compact Fluorescent Light E27: 13 W

6-8
 Materials
Granulated Aluminum Oxide
ZWSK36
dp = 0.425 mm , ps = 1830 kg/m3
ZWSK54
dp = 0.250 mm , ps = 1810 kg/m3
ZWSK70
dp = 0.180 mm , ps = 1780 kg/m3
ZWSK100
dp = 0.100 mm , ps = 1760 kg/m3
Particle Density p = 4000 kg/m3

Study Guides
Understand advantages and disadvantages when fluidization is compared with other
similar used unit operations?
Find out more industrial applications of fluidized beds.

Updated
28 Febuary 2022

6-9
 Lab 7: Cooling Tower

1. Introduction
Cooling towers are commonly utilized to remove heat from hot water generated in
industrial processes. Water is distributed in the tower by spray nozzles, splash bars, or
film-type fill, exposing a very large water surface area to flowing air. The air is
circulated by fans, convective currents, natural wind currents, or induction effects
from sprays. Before being discharged into the atmosphere, the high-humidity air is
passed through a drift eliminator to remove the water droplets. In a direct-contact
cooling tower, water is exposed directly to the cooling atmosphere as schematically
shown in Fig. 1.

Fig. 1 Direct-contact or Open evaporative cooling tower [1].

The performance of cooling towers can be expressed in terms of cooling range and
approach. The difference between the entering and the leaving water temperatures is
the cooling range or the range. The limiting temperature at which the water can be
cooled is the wet-bulb temperature of the air entering the tower. The difference
between the leaving water temperature and the wet-bulb temperature of the entering
air is the approach to the wet bulb or the approach.

7-1
2. Objectives
Select the appropriate flow rate of air for the specific inlet water flow rate and
temperature.

3. Theory
3.1. Fundamental principles
The temperature of the water is reduced in a cooling tower by a combination
of heat and mass transfer. A psychrometric analysis of the air flowing through a
cooling tower is illustrated in Fig. 2.

Fig. 2 Psychrometric analysis of air flowing through cooling tower [1].

Air enters a cooling tower at the ambient condition Point A. Since ambient air
partly contains water vapor, the ability of the air to continue absorbing water vapor is
a measure of cooling [2]. The maximum water-absorption capacity of the air is reached
at a relative humidity of 100 %. In addition to moisture, the air also absorbs heat,
leading to a higher dry-bulb temperature. Unless the load is very light, the air will be
discharged from the tower at Point B in a fully saturated condition. The amount of heat
that the air absorbs from water is directly proportional to the difference in the enthalpy
of the leaving and entering the air. As constant enthalpy lines coincide with lines of
constant wet-bulb temperature, the change in enthalpy of the air corresponds to the
change in wet-bulb temperature of the air. The heat transferred to the air can be broken
down into two components. AC line represents the sensible heat absorbed by the air.
CB line represents the latent heat portion.

7-2
 Despite the same total heat transfer, the sensible and latent heat components
will significantly change if the entering air condition is changed to point D, which has
the same wet-bulb temperature as that of Point A but is at a higher dry-bulb
temperature. In this case, the air is cooled by the sensible heat transfer, which is
represented by the DE line. The latent heat transfer is represented by the EB line.
The temperature of water decreases rapidly in the upper portion of the tower
[2]. Toward the bottom, it changes less rapidly. The temperature gradient in water at
the top part of a cooling tower falls from the bulk of water to the water-air interface,
and from the interface to the bulk of air. At the bottom part of a tall tower, the water
temperature can be higher than the temperature of the air. The temperature gradient in
water is in the same direction as that of water in the top part, but the temperature
gradient in the air is in the opposite direction, i.e. from the bulk of the air to the
interface.

3.2. Psychrometric chart

A psychrometric chart is a graphical representation of the thermodynamic
properties of air. The chart on the next page is based on a standard barometric pressure
of 101.325 kPa. A state point on the psychrometric chart can be found by the
intersection of two property lines. From the established state point, several other
properties including humidity ratio, relative humidity, specific volume, and the dew-
point temperature of the moist air can be determined.

7-3
Fig. 3 Psychrometric chart [3].

7-4
4. Experiment
The cooling tower unit is shown in Fig. 4 and the arrangement of the sensors and
the other components of the system can be seen from a schematic of the system as
shown in Fig. 5. The factors that can be studied are water flow rate, inlet water
temperature, and air flow rate.

4.1. Procedure
1. Measure thermometer wet-bulb temperature, dry-bulb temperature, and
water temperature, then, analyze the data and discuss with a laboratory
supervisor.
2. Study the cooling tower unit and how to measure its performance. The
range of inlet-water temperature is from 38 to 40 oC. The range of inlet-
water flow rate is from 50 to 90 L/h. The lowest pressure drop of air
flowing in the column is approximately 10 Pa, and the maximum pressure
drop is dependent on an inlet-water flow rate.
3. Develop an experimental design for the data collection. Ensure that the
experimental method reflects the awareness of safety issues.
4. To put the cooling tower into operation, the system must be connected to
the main socket (230V/50 Hz). After the main switch is actuated, only the
displays light up initially.
5. The individual operating modes (fan, pump, and heaters) are put into
operation via separate switches. The temperature controller is actuated
when the system is connected to the main socket, but the heaters will not
be actuated until the heaters are turned on.
6. Instead of the relative humidity values reported by the sensors, wet-bulb
temperatures are used to determine the air properties. For this reason,
students must know how to make a simple wet-bulb thermometer by
using gauze. Furthermore, students must be able to explain the basic
principles of heat and mass transfer occurring between the water
covering the thermometer bulb and the passing air.

7-5
 1. Bench frame 13. Tank with heaters
2. Main switch 14. Air chamber
3. Digital displays 15. Air damper
4. Cooling column 16. Fan
5. Temperature sensor of water inlet 17. Orifice
6. Combined temperature/humidity sensor 18. Cover
7. Injection nozzle 19. Pressure tappings
8. Connection hose 20. Make-up water valve
9. Make-up water tank (Inside diameter = 12.6 cm) 21. Make-up water tank filling plug
10. Water flow rate sensor 22. Water filter
11. Regulating valve 23. Drain valve of water tank
12. Circulation pump 24. Temperature controller

Fig. 4 Schematic of cooling tower unit.

7-6
1. Humidity sensor, air inlet 8. Temperature sensor, make-up tank
2. Temperature sensor, air inlet 9. Volumetric flow sensor (water)
3. Humidity sensor, air outlet 10. Air fan with damper
4. Temperature sensor, air outlet 11. Water pump
5. Differential pressure sensor (normally 12. Regulating valve water
for determining the volumetric flow 13. Water filter
(air)) 14. Cooling column
6. Temperature sensor, water inlet 15. Make-up water tank
7. Temperature sensor, water outlet 16. Temperature controller sensor

Fig. 5 Piping and instrumentation schematic of cooling tower unit.

4.2. Care and maintenance

1. Never switch on the heaters or turn on the pump if the water level in the
heating tank is not above the end of the pipe from the make-up water tank.
The water level in the heating tank is higher than the end of the pipe when
no bubbles are flowing into the make-up water tank.
2. After completing the experiments, the fan should remain in operation to
dry the cooling tower and the drip separator.
3. The cooling tower should be operated with distilled or de-ionized water.
4. The make-up tank must be refilled before the water level falls below
approximately 50 mm.
5. To prevent the growth of algae, the water should be drained if the cooling
tower is not in use for a long period.

7-7
4.3. Calculations [4]
4.3.1. Air mass flow rate
The air mass flow rate can be calculated by using equation 1.

𝑚̇𝐿 = 𝑐√(𝑃1 − 𝑃2 )𝜌 (1)

where 𝑚̇𝐿 = Mass flow rate of dry air (kg/s)

c = 4.3281710−3 m2
P1 - P2 = The pressure drop in the column (Pa)
 = Density of air (kg/m3)

4.3.2. The cooling capacity of the air

The cooling capacity of the air (𝑄̇𝐿 ) can be divided into two parts.

𝑄̇𝐿 = 𝑄̇𝑉 + 𝑄̇𝐾 (2)

where 𝑄̇𝑉 = Cooling capacity as a result of evaporation (kJ/s)

𝑄̇𝐾 = Cooling capacity as a result of convection (kJ/s)

The evaporation share of the cooling capacity (𝑄̇𝑉 ) is obtained with the
following equation:

𝑄̇𝑉 = 𝑚̇𝐿 [∆𝐻

̂𝑣𝑎𝑝 (𝑥2 − 𝑥1 ) + 𝐶𝑃𝑣 (𝑥2 𝑇2 − 𝑥1 𝑇1 )] (3)

where
̂𝑣𝑎𝑝 = Enthalpy of vaporization (kJ/kg)
∆𝐻
𝐶𝑃𝑣 = Specific heat capacity of water vapor (kJ/(kg K))
𝑥1 = Absolute humidity of entering air (kg water/kg dry air)
𝑥2 = Absolute humidity of leaving air (kg water/kg dry air)
𝑇1 = Dry-bulb temperature of entering air (K)
𝑇2 = Dry-bulb temperature of leaving air (K)

7-8
 The share of the cooling capacity that is covered by convection (𝑄̇𝐾 ) is
determined by the following equation:

𝑄̇𝐾 = 𝑚̇𝐿 𝐶𝑃𝐿 (𝑇2 − 𝑇1 ) (4)

where 𝐶𝑃𝐿 = The specific heat capacity of air (kJ/(kg K))

4.3.3. Heat load

Due to some heat losses, the actual heat load (𝑄̇𝑊 ) is not the same as
the energy in warm water flowing out of the heating tank. Therefore,
the heat load is calculated from equation 5.

𝑄̇𝑊 = 𝑉̇𝑊 𝜌𝑊 𝐶𝑃𝑊 (𝑇𝑊1 − 𝑇𝑊2 ) (5)

where 𝑄̇𝑊 = Heat load (kJ/s)

𝑉̇𝑊 = Volumetric flow rate of water (m3/s)
𝜌𝑊 = Density of water (kg/m3)
𝐶𝑃𝑊 = Specific thermal capacity of water (kJ/(kg K))
𝑇𝑊1 = Temperature of the entering water (K)
𝑇𝑊2 = Temperature of the leaving water (K)
Note that 𝜌𝑊 and 𝐶𝑃𝑊 of water should be taken from the mean water
temperature.
The maximum possible heat load is determined based on the wet-bulb
temperature of the entering air as shown by equation 6.

𝑄̇𝑊,𝑚𝑎𝑥 = 𝑉̇𝑊 𝜌𝑊 𝐶𝑃𝑊 (𝑇𝑊1 − 𝑇𝑓1 ) (6)

where 𝑄̇𝑊,𝑚𝑎𝑥 = Maximum possible heat load (kJ/s)

𝑇𝑓1 = Wet-bulb temperature of the entering air (K)

7-9
 4.3.4. Cooling range
The cooling range is the difference between the temperature of the
water entering the column (𝑇𝑊1) and the temperature of the water
leaving the column (𝑇𝑊2).

4.3.5. Wet-bulb approach

The cooling limit temperature of water corresponds with the wet-bulb
temperature of the air entering the column. The wet-bulb approach is
the difference between the temperature of the water exiting the column
(𝑇𝑊2) and the cooling limit temperature or the wet-bulb temperature of
the entering air (𝑇𝑓1 ).

4.3.6. Water loss due to evaporation

In the case of cooling towers with open circuits, a certain water loss is
unavoidable due to the material exchange. The quantity of water
evaporated is calculated by equation 7.

𝑚̇𝑊 = 𝑚̇𝐿 (𝑥2 − 𝑥1 ) (7)

where 𝑚̇𝑊 = Rate of water loss due to evaporation (kg/s)

5. Data analysis, discussion, and conclusions

1. Use experimental data to do all calculations listed in section 4.3.
2. Use all relevant engineering principles, standards, and practices to properly
assess the performance of the cooling tower.
3. Draw the conclusions based on scientific/engineering principles, standards,
and practices.

7-10
6. References
1. Chapter 39 Cooling tower, 2008, ASHRAE Handbook - HVAC Systems and
Equipment.
2. Coulson, J.M. and Richardson J.F., 1977, Chemical engineering, volume 1,
Fluid flow, heat transfer, and mass transfer, 3rd edition, Oxford:
Pergamon, (reprinted 1978).
3. Psychrometric chart - Hands Down Software [online], Available:
http://www.handsdownsoftware.com/nautica-chart.pdf [July 4, 2017].
4. Experimental Instruction WL320 Demo Cooling Tower, G.U.N.T. Gerätebau
GmbH, Germany.

Updated
January 9th, 2024

7-11
 Tubular Flow Reactor

1. Introduction
In the majority of industrial chemical processes, the reactor is the key item of
equipment in that the required chemical change of raw materials to form desired
products occurs at this point of the whole process. The design and operation of
chemical reactors are thus crucial to the whole success of the industrial operations.
Tubular flow reactors are commonly used in the industry. If the flow field in a tubular
reactor is highly turbulent, plug flow assumption is generally made in the design of such
reactors. Due to mixing in the longitudinal direction and incomplete mixing in the
radial direction, deviations from an ideal tubular flow (plug flow) behaviour are
possible. The reaction chosen in this experiment is the saponification of ethyl acetate
(EtOAc) with dilute sodium hydroxide (NaOH):

NaOH + EtOAc NaOAc + EtOH

2. Objectives
1. To determine the rate law using tubular flow reactor data.
2. To understand the various parameters on tubular flow reactor performance
such as flow rate.

3. Experimental
An Armfield CET Tubular Flow Reactor will be used in the experiments. A
tubular reactor of length 22 m. and volume 0.4 L. is placed in a constant temperature
water bath. Temperature of the reactor was adjusted to the desired value by controlling
the water bath temperature which is heated by heating elements. Two feed tanks contain
the reactants which are pumped by the two positive displacement type pumps through
the flowmeters into the inlet feed pipes where they enter the reactor coil. The mean
residence time in the coil is a function of the flowrate, set by the flowmeters. Control of
the equipment which is situated on the front panel, is governed by a mains on/off switch,
pump switches, a temperature scale and stirrer motor switch.
3.1 Equipment and Chemicals
1. Flasks
2. pipette
3. burette
4. graduate cylinder
5. 0.05 M NaOH
6. 0.05 M HCl
7. 0.05 M EtOAc
8. phenolphthalein indicator

3.2 Procedures
1. Before experiment, answer/discuss the following questions.
- How can you analyze reactants and products of a saponification reaction
by titration?
- Derive the design equation of a plug flow reactor.
- Discuss the experimental parameters for rate law (rate constant and rate
order in PFR) determination.
2. Carry out the reaction in tubular reactor by using selected equal molar
flowrates of the reactants.
2. Follow the reaction by analyzing outlet concentrations of NaOH at different
consecutive times until steady state.
3. Repeat these experiments at 4 different space times.

4. Data Analysis and Discussion

1. Determine the fractional conversion values in each experiment.
2. Discuss the effect of flow rate on conversion values.
3. Determine the reaction order and rate constants.

5. References
1. Smith, J.M., 1981, Chemical Engineering Kinetics, McGraw Hill Int.
2. Fogler, H.S., 1992, Elements of Chemical Reaction Engineering, 2nd
Edition, Prentice-Hall Inc., USA.
3. Levenspiel, O., 1972, Chemical Reaction Engineering, 2nd Edition, John
Wiley and Sons, New York.
4. Armfield CET-Tubular Flow Reactor, 1993, Instruction Manual.