(KMK20303) Lab Module Sem 1 20232024

LABORATORY
MODULE
KMK20303/3
REACTION ENGINEERING
SEMESTER 1 (2023/2024)
En. Zulkarnain Bin Mohamed

Idris
Dr. Noor Hasyierah Binti Mohd
Salleh
Dr. Azalina Binti Mohd Nasir
Cik Khalilah Mohamad Yusuff
Faculty of Chemical Engineering

Technology
University Malaysia Perlis

CONTENT
CONTENT ii
CLEANLINESS AND SAFETY iii
LABORATORY GUIDELINE v
EXPERIMENT 1 : INTRODUCTION TO THE LABORATORY SAFETY 1
EXPERIMENT 2 : EFFECT OF FLOW RATE ON THE REACTION 1

IN A CONTINUOUS STIRRED TANK REACTOR
(CSTR)
EXPERIMENT 3 : EFFECTS OF FLOW RATE AND REACTION 8

TEMPERATURE ON CONVERSION IN A TUBULAR
REACTOR
EXPERIMENT 4 : DETERMINATION OF REACTION RATE 15

CONSTANT AND REACTION ORDER IN BATCH
REACTOR
EXPERIMENT 5 : EFFECT OF TEMPERATURE ON REACTION 27

AND REACTION’S ACTIVATION ENERGY FOR
BATCH REACTOR.
EXPERIMENT 6 : EFFECT OF RESIDENCE TIME ON 40

THE REACTION IN CATALYTIC TUBULAR
REACTOR
EXPERIMENT 7 : EFFECT OF PULSE CHANGE IN INPUT 51

CONCENTRATION TO THE
CONCENTRATION OF SOLUTE IN STIRRED
TANK REACTOR (CSTR) IN SERIES
iii
CLEANLINESS AND SAFETY
CLEANLINESS
The Reaction Engineering Laboratory contains equipment that uses water or

chemicals as the fluid. In some cases, performing an experiment will unavoidably
allow water/chemicals to get on the equipment and/or on the floor.
There are “housekeeping” rules that the user of the laboratory should be aware and
abide by. If no one cleaned up their working area after performing an experiment, the
lab would not be a comfortable or safe place to work in. Consequently, students are
required to clean up their area at the conclusion of the performance of an
experiment. Cleanup will include
 removal of spilled water (or any liquid) or chemicals

 wiping the table top on which the equipment is mounted
The lab should always be as clean as or cleaner than it was when you entered.
Cleaning the lab is your responsibility as a user of the equipment.
SAFETY
This is to serve as a guide and not as a comprehensive manual on safety. Every
staff/student has, at all time, a duty to care for Health and Safety of himself/herself
and of all people who may be affected by his/her action.
PROTECTIVE CLOTHING – Lab coat MUST be worn all times. Rubber gloves
should be worn when handling corrosive materials, and heat-proof gauntlets when
discharging any equipment involving heat.
FOOTWARE – Wear fully covered shoes with strong grip.
EYE PROTECTION – Goggles must be used whenever necessary especially when

dealing with high pressure equipment.
iv
ELECTRICITY – Sometimes the floor may be wet. Therefore, care is essential.
Always switch off power before removing plugs from sockets.
CABLES AND HOSES – Cables must be suspended and not lying on the floor. All
cables and hoses should be routed to avoid walk-ways.
BROKEN GLASS – This should be disposed off in the glass bin, not in the usual
waste bin. Breakage should also be reported to the Instructor in charge.
INSTRUCTION SHEETS – Any appropriate instruction sheets should be studied

before starting the experiment. Particular attention should be given to the
recommended precautions, start-up procedure and sequence of operation.
There should be NO EATING in the laboratory. Smoking is strictly prohibited in all

laboratories.
In case of emergency, report to the Instructor in charge or

doctor/ambulance/fire fighter from:
Hospital Tuanku Fauziah, Kangar 04-9763333

Bomba Perlis 04-9778827
SAFETY FIRST
iv
LABORATORY GUIDELINE
BRING ALONG:
 Lab manual
 Lab coat
 Shoes (no sandals are allowed)
 Neat and suitable clothes
 Necessary stationeries (calculator, pen, marker pen…)
 Lab Report (Front cover, Objectives, Flowchart, Lab sheet)
MUST:
 Discipline – punctual
 Ready for the experiment – read and understand the procedures
 Be in group and gather at the experiment station as scheduled
 Participate in the lab activity.
 Submit the result data (to be stamped by lecturer/teaching engineer) by end of
each lab session
v
PTT 255/3 – Reaction Engineering Laboratory Module
EXPERIMENT 1
INTRODUCTION TO THE LABORATORY SAFETY
1.0 OBJECTIVE
1.1 To identify applicable safety measures in performing the reaction engineering

laboratory practice.
1.2 To determine the necessary precautions prior to usage of reaction engineering
learning apparatus.
2.0 COURSE OUTCOME
CO1: Ability to DEMONSTRATE the principles of chemical reaction engineering design for
industrial reactors.
3.0 INTRODUCTION TO LABORATORY SAFETY
The Engineering Laboratory contains equipment that use chemicals and water as the fluid. In
some cases, performing an experiment will inevitably allow water and chemicals to get on the
equipment and/or on the floor. Thus, the most basic practice in maintaining safe working
environment is to ensure that the workplace is well kept clean and organized at all times.
Laboratory users are required to clean up their work area at the end of every experiment
performed. Cleanup will include, but not limited to, removal of spilled liquid and wiping the table
top on which the equipment is mounted. However, it is imperative that the lab should always be
kept clean as practicably possible, even during the experimental run.
Beside cleanliness, the use of personal protection equipment (PPE) is also vital to ensure one’s
safety during the experimental run. PPE is considered as the last resort protection and should be
selected appropriately. PPE must be properly fitted, tested, cleansed, maintained and stored.
Comfortable PPE will ensure the efficiency of its usage towards protecting the users from specific
hazards.
1
PROTECTIVE CLOTHING – Lab coat MUST be worn all times. Rubber gloves should be worn
when handling corrosive materials, and heat-proof gauntlets when discharging any equipment
involving heat.
FOOTWARE – Wear fully covered shoes with strong grip.
EYE PROTECTION – Goggles must be used whenever necessary especially when dealing with
high pressure equipment.
ELECTRICITY – Sometimes the floor may be wet. Therefore, care is essential. Always switch off
power before removing plugs from sockets.
CABLES AND HOSES – Cables must be suspended and not lying on the floor. All cables and
hoses should be routed to avoid walk-ways.
BROKEN GLASS – This should be disposed off in the glass bin, not in the usual waste bin.
Breakage should also be reported to the Instructor in charge.
INSTRUCTION SHEETS / LAB PROCEDURES – Any appropriate instruction sheets or lab

procedures should be studied before starting the experiment. Particular attention should be given
to the recommended precautions, start-up procedure and sequence of operation.
3.1 REACTOR ENGINEERING LEARNING APPARATUS
The apparatus for the reaction engineering laboratory is listed as follows:

i. Continuous-Stirred Tank Reactor
ii. Tubular Flow Reactor
iii. Batch Reactor
iv. Catalytic tubular reactor
v. Continuous stirred tank reactor (CSTR) in series.
4.0 EXPERIMENTAL PROCEDURES
1. Locate each reaction engineering apparatus provided in the laboratory.

2. Based on the physical appearance of the apparatus, assembly of equipment such as
pumps and tanks, and connections of piping, fittings and gauges at each apparatus:
a) Identify the necessary PPE to be utilized during the experimental run.
1
b) Analyze all safety sign in the laboratory.
c) Develop the general start-up and shutdown procedures as well as other necessary
precautions for the apparatus.
5.1 RESULTS AND DISCUSSIONS
1. Write the general lab procedures in Reaction Engineering Lab

2. Present your findings in section 4.0 (No.2) in a tabulated manner.
3. Discuss the first aid measures for each chemical that you will used in the laboratory (Refer
to Material Safety Data Sheet, MSDS).
6.0 CONCLUSION
Conclude your findings related to importance of laboratory safety.
2
EXPERIMENT 2
EFFECT OF FLOW RATE ON THE REACTION IN A CSTR
1.0 OBJECTIVE
1.1 To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
1.2 To determine the effect of flow rate on the extent of conversion.
2.0 CORRESPONDING COURSE OUTCOME

CO 1- Ability to DEMONSTRATE the principles of chemical reaction engineering design for
3.0 INTRODUCTION
The Continuous Stirrer Tank Reactor Unit-Single (CSTR-Single), Model: K1041 has
been designed to allow students to investigate reactor and reaction behaviour. The unit comes
complete with a glass reactor, individual reactant feed tanks and pumps, temperature sensors and
conductivity measuring sensor. The reactor will enable students to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide among other types of
reaction.
CSTR is the most basic of the continuous reactors used in chemical process, which is used
primarily for liquid phase reaction. It also known as vat– or backmix reactor. It is an open system,
where material is free to enter or exit the system, and it also operates on a steady basis, where
the conditions in the reactor do not change with time. In CSTR, reactants are continuously
introduced into the reactor, while products are continuously removed. Solution in CSTR is assume
well–mixed, which has relatively uniform properties such as temperature and density.
4.0THEORY
From the general mole balance equation on a CSTR (Figure 1),
Eq. (1)
So, the design equations for the continuous-stirred tank reactor.
Eq. (2)
3
Figure 1: Mole balance on a CSTR
In chemical reactions, it is often that one of the reagents deplete before the others.
When this occurs, the reaction ceases, and thus this reagent is termed the limiting reagent. In
most instances, it is best to choose the limiting reagent as the basis of stoichiometric
calculations. Consider a general reaction
Eq. (3)
where the uppercase letters represent chemical species, and the lowercase letters represent
stoichiometric coefficients (moles). Suppose that species A were to be the limiting reagent, we
then divide the reaction expression by the coefficient of species A, to obtain
Eq. (4)
Now that the other chemical species are on a “per mole of A” basis, we would then want to know
how far the reaction proceeds to the right, or how many moles of A are consumed to form one
mole of C. These can be determined by defining a parameter called conversion. The conversion
of chemical species A is simply the number of moles of A that have reacted per mole of A fed into
the system.
Eq (5)
4
Now that we understand the basic chemistry and chemical engineering involved in
chemical reactors, consider a chemical reaction between an ether and sodium hydroxide. This
process is also known as saponification. The reaction is reversible, and is described by
The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules;
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress of the
reaction can thus be tracked accurately by the change in hydroxide ions. This can be observed by
the conductivity change in the reactor vessel, since the presence of hydroxide ions increase the
conductivity in a solution.
5.0 MATERIALS AND EQUIPMENT
5.1 Description of Apparatus

The unit comes with all the ancillary equipment except analytical
instrumentation for the measurement of the composition of feed and product
mixtures. All necessary instruments are fitted at suitable locations for the
measurements of the reaction temperature, reactant flow rates and conductivity.
The SCADA system is supplied, which allows real time monitoring and data
logging of all sensor outputs. The unit includes a reactor vessel of approximately 10
liters total capacity and equipped with a variable speed stirrer with digital display,
inlet and outlet ports for the feed and product streams, sampling, temperature
measurement and control. Two non-corroding feed storage vessels are supplied,
together with peristaltic pump. A digital temperature controller is also provided on
the front panel. A conductivity meter is provided for the purpose of determining the
extent of conversion.
5.2 Description and Assembly

Before operating the unit and running experiments, students must familiarize
themselves with every components of the unit. Please refer to Figure 2-3 and
Table 1 to understand the process.
5
Figure 2: CSTR reactor-Front view.
Figure 3: CSTR reactor-Back view.
6
a. Overall Dimension
Height : 2.00 m
Length : 1.00 m
Width : 0.80 m
b. Reactor (R-101)
Material : Borosilicate glass; stainless steel top and bottom plate
Total Volume : 8 liters
Working Volume : 5 liters
Cooling System : Cooling water through stainless steel cooling coil
Heating System : 1.5 kW; immersion heater; Temperature Sensor;
Equipped with :Feed inlets, temperature transmitter, conductivity transmitter,
sampling/drainage, overflow tube
c. Stirrer System
Variable Speed : 50 to 2200 rpm; with speed controller and LCD indicator
Impellers : 2” diameter; stainless steel
Electrical : 240VAC/1-phase/50-60Hz
d. Feed Tank (T-101, T-102)

Capacity :20 liters (Cylindrical)
Material : Stainless Steel
e. Product Tank (T-103)

Capacity : 60 liters (cylindrical)
Material : Polyethylene (PE)
f. Feed Pump (P-101, P-102)

7
Type : Peristaltic
Speed : 0 to 600rpm
Flowrate : 0 to 2.28 L/min
g. Conductivity Meter (AT-101)

Range : 0 to 2000 μS/cm
Output : 4 to 20 mA
h. Temperature Transmitter (TT-101)

Type : RTD, Pt100
Range : 0 to 100°C
i. Control Panel
All necessary electrical components and data acquisition modules are housed in
the control panel. Instrumentations and digital displays are panel mounted.
j. Valves List
Valves list:
6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conversion vs Conductivity.

a. Prepare the following solutions:
i) 6 bottles of 0.5L of 0.010M of Sodium Hydroxide, NaOH
ii) 1 bottle of 0.5L of 0.002M of Ethyl Acetate, Et(Ac)
iii) 1 bottle of 0.5L of 0.004M of Ethyl Acetate, Et(Ac)
iv) 1 bottle of 0.5L of 0.006M of Ethyl Acetate, Et(Ac)
v) 1 bottle of 0.5L of 0.008M of Ethyl Acetate, Et(Ac)
vi) 1 bottle of 0.5L of 0.010M of Ethyl Acetate, Et(Ac)
b. Mix the solutions according to Table 2 as shown.
8
6.2 Start up
1. Switch on the main power supply.

2. Switch on Isolation switch by rotating clockwise.
3. Switch on “main switch” by rotating clockwise.
4. Turn on the tablet by pressing the button at the top left of the tablet.
5. Double click the SIMATIC WinCC icon at the left of the desktop.
9
6. Then, click the “Play” icon (Blue) at the top left of the software and SCADA
Graphic main page will be appeared.
7. Make sure the Wi-Fi icon is green colour, indicates the system is connected.
6.3 Experiment Effect of Flow Rate On The Reaction In A CSTR
1. Prepare and charge 20 L of 0.01M Ethyl Acetate (Et (Ac)) solution into feed tank T-
101.
2. Prepare and charge 20 L of 0.01M Sodium Hydroxide (NaOH) solution into feed
tank T-102.
3. Open valve V-108.
4. Switch on pumps P-101 and P-102 simultaneously by pressing on the “P101 ON”
and “P-102 ON” push button on the local control panel.
5. Adjust the speed to 260 rpm (equivalent to 1.0 LPM) respectively.
6. Once set the speed, close valve V-108.
7. Fill up the reactor vessel until it is just about to overflow.
8. Switch on stirrer and set the stirrer speed to approximately 600 rpm..
9. Start the stopwatch.
10. Record conductivity readings according to AI-101 on the local control panel every
minute until it reaches steady state.
11. Repeat the experiment with a speed of 200 rpm and follow by 140 rpm without switch
off the pumps (P- 101& P-102)
10
6.4 Shut Down
1. Adjust the pumps speed to 260rpm.

2. Switch off pumps (P-101 and P-102).
3. Switch off stirrer (M-101).
4. Switch off the SCADA by pressing the top left “X” button.
5. Click “EXIT” on the pop out dialogue.
6. Switch off the power supply at the control panel.

7. Open valves V-102 and V-104 to drain all the solutions from feed tanks T-101 and T-
102. Otherwise, close valves V-102 and V-104 to keep the solutions for subsequent
experiment.
8. Open V-106 & V-108 to drain any solution from the reactor R-101 and store any
solution needed in a proper labelled container. Consult the lab technician regarding
11
chemical storage.
9. Fill the feed tanks with 10L of tap water respectively and switch on both P-101 and P-
102.
7. Flush the system with tap water for few minutes and then drain and dispose of the
water down the drain.
8. Open valve V-107 to drain any solution from the product tank T-103.
9. Properly dispose of any unwanted material, consult the lab technician for guidance.
10. Fill the feed tanks with 5L of distillate water respectively and switch on P-101 and
P-102.
11. Fill up the reactor tank with distillate water until 5L to protect the heater, temperature
and conductivity sensor.
12. Close all the valves.
7.0 RESULTS
7.1 Record all the results in appropriate tables.
7.2 Plot graph of conversion vs. conductivity.
7.3 Plot a graph of conversion vs. time for every flow rate.
8.0 DISCUSSION
8.1 Discuss the effect of flow rate on the conversion.
8.2 Discuss appropriate discussion regarding this experiment.
9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.
12
APPENDIX A1: Physical Properties of Et(Ac) and NaOH.
Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH
Formula CH3COOCH2CH3 NaOH
Appearance clear liquid white solid
Molecular weight 88.11 g/mol 40.00 g/mol
Normal boiling point 77.1°C 1390° C
Normal melting point -84.0°C 323°C
Density 0.8945 g/mL @ 25°C 2.1 g/mL
Refractive index 1.3274 @ 20°C –
APPENDIX B1: Effect of flow rate on conductivity and conversion over time.
13
EXPERIMENT 3
EFFECTS OF FLOW RATE AND REACTION TEMPERATURE ON

CONVERSION IN TUBULAR REACTOR
1.0 OBJECTIVE
1.1 To observe and control the operation of a tubular reactor.
1.2 To determine the effects of flow rate and reaction temperature on conversion in a
tubular reactor.
CO 1- Ability to DEMONSTRATE the principles of chemical reaction engineering design for

3.0 INTRODUCTION
The tubular reactor, also known as the plug flow reactor (PFR) is a type of continuous flow
reactor commonly used in industrial processing. As with all continuous flow reactors, PFRs
are almost always operated at steady state. In tubular flow reactor, one or more fluid
reagents are pumped through a pipe or tube. As the reactants flow down the length of the
reactor in a PFR, they are continually consumed. When modeling a tubular reactor, it is
assumed that the concentration varies continuously in the axial direction through the
reactor. Subsequently, the reaction rate also varies axially, since it is a function of
concentration (except for zero-order reactions). Now, consider a system which the flow
field is modeled by that of a plug flow profile (uniform velocity as in turbulent flow).
Thus, there should be no radial variation in reaction rate, as shown in Figure 1.
Figure 1: Plug-flow tubular reactor
14
4.0 THEORY
4.1 Conversion In Tubular Reactors
General mole balance equation:
There are two ways we can use to develop a design equation for the PFR; the first involves
differentiating the general mole balance equation with respect to volume V,
while the second method is by performing a mole balance on species j in a small volume ΔV (as
shown in Figure 2). For the second method, the differential volume will be chosen such that there
are no spatial variations in reaction rate within this volume.
Figure 2: Mole balance on species j in a differential volume ΔV
The generation rate, ΔGj would then be
15
4.2 Saponification of Ethers with Sodium Hydroxide

Now that we understand the basic chemistry and chemical engineering involved in
chemical reactors, consider a chemical reaction between an ether and sodium hydroxide.
This process is also known as saponification.
The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules,
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress of
the reaction can thus be tracked accurately by the change in hydroxide ions. This can be
observed by the conductivity change in the reactor vessel, since the presence of hydroxide
ions increase the conductivity in a solution. As the conversion increases, the hydroxide
ions depletes to form ethanol, and this should be observed by a decrease in conductivity.
5.1 Description of Apparatus

The Tubular Flow Reactor (Model: K1081) is designed for students of Chemical
Engineering to observe the behaviour of a “plug flow” reactor by studying the second
order reaction between dilute caustic soda and ethyl acetate. The unit is small in scale for
ease of operation but capable of demonstrating the principles of industrial scale reactor
behaviour. The unit includes a 11-liter reactor vessel as a water jacket, and is equipped
with a variable speed stirrer, inlet and outlet ports for the feed and product streams,
sampling, conductivity measurements and temperature measurements and control.
This unit comes with all the ancillary equipment except analytical instrumentation for the
measurement of the composition of feed and product mixtures. All necessary instruments
are fitted at suitable locations for the measurements of the reaction temperature, reactant
flow rates and conductivity. All the sensors are of electronic type to ensure compatibility
with data acquisition system. The SCADA system is supplied, which allows real time
monitoring and data logging of all sensor outputs.
A cooling coil and immersion heater are provided inside the vessel to provide constant
reaction temperature. The desired reaction temperature is achieved by controlling the
heating using a digital temperature controller located on the front panel. Two non-
corroding feed storage vessels are supplied, together with peristaltic feed pump. A
product collection vessel is also provided and if necessary, the products are neutralised
before discharging to the laboratory drains.
The tubular reactor is a coil of long tubing wound around a cylinder inside the vessel to
give a total reactor volume of approximately 0.4 liters. The spiral design is practically the
best approximation to plug flow conditions, as the secondary flow ensures good radial
mixing while minimizing longitudinal dispersion. The two reactants are pre-heated prior
for mixing and entering the reactor.
5.2 Description and Assembly

Before operating the unit and running experiments, students must familiarize
themselves with every components of the unit. Please refer to Figure 3-4 and
Table 1 to understand the process.
16
Figure 3: Reactor-Front view.
Figure 4: Reactor-Back view.
17
a. Overall Dimension
Height : 2.10 m
Depth : 0.80 m
Width : 0.95 m
b. Reactor (R-101)
Water Jacket : 11 liters; borosilicate glass; stainless steel top and bottom plate
Cooling System : 3/8” stainless steel tube with connections for cooling water
Heating System : 1.0 kW immersion heaters; temperature sensor; temperature
controller
Tubular Reactor : 2.0m long and 8mm diameter coiled tubing to give a total
reactor volume of approximately 0.4 liters.
Pre-heating : 3 liters stainless steel vessel with coils and circulation pump
c. Stirrer System
Variable Speed : 50 to 2200 rpm; with speed controller and LCD indicator
Impellers : 2” diameter; stainless steel
Electrical : 240VAC/1-phase/50-60Hz
d. Feed Tank (T-101, T-102)

Capacity : 20 liters (Cylindrical)
18
e. Product Tank (T-103)
f. Feed Pump (P-101, P-102)

Type : Peristaltic
Speed : 0 to 600rpm
Flowrate : 0 to 2.28 L/min
g. Conductivity Meter (AT-101)

Range : 0 to 2000 μS/cm
Output : 4 to 20 mA
h. Temperature Transmitter (TT-101 & TT-102)

Type : RTD, Pt100
Range : 0 to 100°C
i. Control Panel
All necessary electrical components and data acquisition modules are housed in
the control panel. Instrumentations and digital displays are panel mounted.
j. Valves List
Valves list:
19
6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conversion vs Conductivity.

a. Prepare the following solutions:
iv) 6 bottles of 0.5L of 0.010M of Sodium Hydroxide, NaOH
iv) 1 bottle of 0.5L of 0.006M of Ethyl Acetate, Et(Ac)
b. Mix the solutions according to Table 2 as shown.
6.3 Start up
1. Switch on the main power supply.

2. Switch on Isolation switch by rotating clockwise.
3. Switch on “main switch” by rotating clockwise.
4. Turn on the tablet by pressing the button at the top left of the tablet.
5. Double click the SIMATIC WinCC icon at the left of the desktop.
20
6. Then, click the “Play” icon (Blue) at the top left of the software and SCADA
Graphic main page will be appeared.
7. Make sure the Wi-Fi icon is green colour, indicates the system is connected.
6.4 Experiment (a) Effect of Flow Rate on The Reaction In A Tubular Reactor.
1. Prepare and charge 20 L of 0.01M Ethyl Acetate (Et (Ac)) solution into feed tank T-
101.
2. Prepare and charge 20 L of 0.01M Sodium Hydroxide (NaOH) solution into feed
tank T-102.
3. Switch on pumps P-101 and P-102 simultaneously by pressing on the “P101 ON”
and “P-102 ON” push button on the local control panel.
4. Adjust the speed of both pumps to 260 rpm (equivalent to 1.0 LPM) simultaneously.
5. Switch on stirrer and set the stirrer speed to approximately 600 rpm.
21
6. Observe the flow of reactant in silicone tubing.
7. Observe and record the highest value of AI-101 on the local control panel.
8. Start the stopwatch.
10. Repeat the experiment with a speed of 200 rpm and follow by 140 rpm without switch
off the pumps (P- 101& P-102)
6.5 Experiment (b) Effect of Temperature on The Reaction In A Tubular Reactor
1. Repeat the experiment with same speed of 200 rpm without switch off the pumps (P-
101& P-102) for temperature of 40°C by following the steps:
i. Click “TRENDS” on the SCADA
ii. Click “TT-102 CONTROL” on the SCADA
22
iii. Input the “SETPOINT” temperature as 50°C. (always set setpoint of TT-
102 10°C higher than setpoint of TT-101.)
iv. Click “TT-101 CONTROL” on the SCADA
v. Input the “SETPOINT” temperature as 40°C.
23
2. Switch on HTR-101 & HTR-102 by pressing ‘HTR101 ON’ & ‘HTR102 ON’ on the
local control panel.
3. Switch on P-103 by pressing ’P103 ON’ on the local control panel to recirculate the hot
water in pre-heat tank T-104 in order to heat up the water evenly.
4. Observe the temperature according to TI-101 & TI- 102 (on the local control panel)
and “TT-101” & “TT- 102” on the SCADA main page.
5. Wait until temperature of the Tl-101 reached 40oC
6. Start timer on the stopwatch.
8. Repeat the experiment for step 1 to 7 for temperature of 50°C.
6.6 Shut Down
1. Adjust the pumps speed to 260rpm.

2. Switch off heater HTR-101 & HTR-102.
3. Switch off pumps (P-101, P-102 and P-103).
4. Switch off stirrer (M-101).
5. Switch off the SCADA by pressing the top left “X” button.
24
6. Click “EXIT” on the pop out dialogue.
10. Switch off the power supply at the control panel.

11. Open valves V-102 and V-104 to drain all the solutions from feed tanks T-101 and T-
102. Otherwise, close valves V-102 and V-104 to keep the solutions for subsequent
experiment.
12. Fill the feed tanks with 10L of tap water respectively and switch on both P-101 and P-
102.
13. Flush the system with tap water for few minutes and then drain and dispose of the
water down the drain.
14. Open valve V-106 to drain any solution from the product tank T-103.
15. Properly dispose of any unwanted material, consult the lab technician for guidance.
16. Fill the feed tanks with 5L of distillate water respectively and switch on P-101 and
P-102.
17. Fill up the reactor tank with distillate water until 5L to protect the heater, temperature
18. Close all the valves.
25
7.0 RESULTS
7.1 Record all the results in the table (Appendix B3) for every reading taken by
conductivity and temperature meter.
7.2 Plot calibration curve graph. (Conversion vs. Conductivity).
7.3 Plot a graph of conversion vs. time for all experiments.
8.0 DISCUSSION
8.1 Discuss the effect of flow rate and temperature on conversion through appropriate
graphs.
9.0 CONCLUSION
26
APPENDIX B1: Effect of flow rate on conductivity and conversion over time.
Feed rate
Time 260 rpm (= 1.0 LPM) 200 rpm (= 0.75 LPM) 140 rpm (= 0.5 LPM)
(min) Condutivity Conversion Condutivity Conversion Condutivity Conversion
(μS/cm) (%) (μS/cm) (%) (μS/cm) (%)
0
1
2
3
4
5
APPENDIX B2: Effect of temperature on conductivity and conversion over time.
Temperature
Time T = room temp T = 40 °C T = 50 °C
(min) Condutivity Conversion Condutivity Conversion Condutivity Conversion
(μS/cm) (%) (μS/cm) (%) (μS/cm) (%)
0
1
2
3
4
5
27
EXPERIMENT 4
Determination of Reaction Rate Constant and Reaction Order in Batch
Reactor
1.0 OBJECTIVES
1.1 To observe and control the operation of a batch reactor for saponification reaction
between Sodium Hydroxide and Ethyl Acetate.
1.2 To determine the reaction rate constant and reaction order in batch reactor.
CO2: Ability to ANALYZE and solve various problem related to reactor design
and reaction process.
3.0 INTRODUCTION
In the majority of industrial chemical processes, reactor is the key equipment in which raw
materials undergo a chemical change to form desired products. The design and operation
of chemical reactors is thus crucial to the whole success of an industrial process. Reactors
can take a widely varying form, depending on the nature of the feed materials and the
products. Understanding the behavior of how reactors function is necessary for the proper
design, control and handling of a reaction system. Two main types of reactors are batch
reactor and continuous flow reactor.
The Reactor Basic Unit (Batch Reactor) has been designed for students‟ experiments on
chemical reactions in liquid phase under isothermal and adiabatic conditions. The unit
comes complete with a glass reactor, constant temperature water circulating unit,
temperature and conductivity measurements. Student shall be able to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide.
28
4.1 THEORY
4.2 Rate of Reaction and Rate Law.
The rate at which a given chemical reaction proceeds can be expressed in several ways. It
can be expressed either as the rate of disappearance of the reactants, or the rate of
formation of products. In the following reaction,
aA + bB cC + dD [1-1]
A and B are the reactants, while C and D are the products. a, b, c, d are the
stoichiometric coefficients for the respective species. If species A is considered as the
reaction basis, then the rate of reaction can be represented by the rate of disappearance
of A. It is denoted by the symbol –rA. The numerical value of the rate of reaction, –rA is
defined as the number of moles of A reacting (disappearing) per unit time per unit volume,
and has the typical unit of mol/dm3.s.
Similarly, the rate of reaction can also be represented by the rate of disappearance of
another species, such as –rB and the rate of formation of a product, such as rC or rD. They
can be related in the following equation,
 rA r rC rD
B
a  b  c  d
[1-2]
4.3 Conversion
Using the reaction shown in Equation [1-1], and taking species A as the basis of calculation,
the reaction expression can be divided through by the stoichiometric coefficient of species A,
in order to arrange the reaction expression in the form,
b c d
A+ B  C + D [2-1]
a a a
The expression has now put every quantity on a „per mole of A‟ basis.
A convenient way to quantify how far the reaction has progressed, or how many moles of
products are formed for every mole of A consumed; is to define a parameter called
conversion. The conversion XA is the number of moles of A that have reacted per mole of
A fed to the system,
moles of A reacted
X A  [2-2]
moles of A fed
29
Because the conversion is defined with respect to the basis of calculation (species A), the
subscript A can be eliminated for the sake of brevity and let X = XA .
4.4 General Mole Balance Equation

To perform a mole balance on any system, the system boundaries must first be specified.
The volume enclosed by these boundaries will be referred to as the system volume. In this
example, a mole balance will be performed on species j in a system volume, where species j
represents the particular chemical species of interest.
Fj0 Fj
Figure 1: Balance on the system volume.
A mole balance on species j at any instant in time, t, yields the following equation,
Rate of j Rate of j  Rate of j   Rate of j 

into   out of   produced   accumulated 
    
system  system  within system within system
       
volume  volume   volume   volume 

in – out + generation = accumulation
dNj
Fj0 – Fj + Gj = [3-1]
dt
where Nj represents the number of moles of species j in the system at time t.
30
Figure 2: Unit construction for Batch reactor
31
Table 1: List of valves.

Description
Tag Location
V-101 Discharge Valve from T-101 to R-101
V-102 Drain Valve of T-101
V-105 Drain valve of R-101
V-106 Drain valve from T-103
V-107 Discharge Valve from T-104 to Heating Coil
Height : 1.50 m
Overall Dimension
Width : 1.10 m
Depth : 0.80 m
General Working Area : Ventilated, approximately 10m2

Requirement
Chemical : Ethyl Acetate & Caustic Soda (0.1M)
are suggested
Utility : 1. Electrical supply: 230VAC, 1-

phase, 50Hz
2. Water: Laboratory main supply with
drainage
32
The Reactor Basic Unit (Batch), Model: K1051)

includes the following items:
Specifications
a) Bench
A bench constructed from aluminium frame and
chemically resistant worktop, comes with lockable
castor wheels.
b) Reactor (R-101)
Reactor Vessel : Borosilicate glass; top and bottom
plate made of non-corroding material
Reactor Volume : 5 liters
Heating System : Heating Coil
Ports : Feed inlets, temperature transmitter,
conductivity, drainage
c) Stirrer System (M-101)

Variable Speed : 50 to 2200rpm; with speed
controller and indicator
Impellers : 50mm diameter, stainless steel
Electrical : 240VAC/1-phase/50-60Hz/50W
d) Feed Tanks (T-101, T-102)

Material : Stainless steel
e) Product Tank (T-103)

33
f) Hot Water Tank (T-104)

g) Feed Pumps (P-101, P-102)

Type : Peristaltic
Capacity : 1 L/min
h) Water Feed Pump (P-103)

Type : Centrifugal
Max Pressure Head : 15m
i) Flow Control (FI-101)

Type : Rotameter
Control valve : Needle valve
Range : 0.5 - 4LPM
j) Conductivity Meter (QT-101)

Sensor range : 0 to 200 mS/cm
Output : 4 to 20 mA
k) Temperature Transmitter
(TT-101, TT-103 & TT-104)
Type : RTD, Pt100
Range : 0 - 100 °C
l) Control Panel
All necessary electrical components and data
acquisition modules are housed in the control panel.
Instrumentations and digital displays are panel
mounted.
34
6.1 PROCEDURES
6.2 Preparation of Calibration Curve for Conductivity vs. Conversion.
6.2.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O
6.2.2 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.
0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL
Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
100% conversion : 100 mL Na(Ac)
6.2.3 Tabulate all data in the table of Appendix B3.
6.3 General Start-up Procedures
6.3.1. Perform a quick inspection to make sure that the equipment is in proper
working condition.
6.3.2. Ensure that all valves are initially closed and all power supply switch are turn
off.
6.3.3. Switch on the main power and power switch on the control panel.
6.3.4. Open valves V-101 and V-103.
6.3.5. The equipment is now ready to use.
6.4 Experimental procedure

6.4.1 Prepare 8L of 0.1M NaOH and Et(Ac) solution into respective feed tank T-
101 and T-102.
6.4.2 Switch on the pump P-101 to charge 1L of NaOH into the reactor tank.
6.4.3 Switch off the pump P-101 and close the inlet valve (refer to Figure A1) and
switch on conductivity meter (QT-101) on the control panel.
6.4.4 Switch on pump P-102 to charge 1L of Et(Ac) into the reactor tank, which
make up a total 2L of solution in the reactor.
6.4.5 Switch off the pump P-102 and close the inlet valve (refer to Figure A1).
6.4.6 Switch on stirrer (M-101) on the control panel. Set the stirrer speed to
approximately 500 rpm.
35
6.4.7 Record the initial conductivity value (QI-101).
6.4.8 Start the stopwatch immediately.
6.4.9 Start monitoring and record the conductivity value (QI-101) in Table of
Appendix C3 for every 10 seconds.
6.4.10 Stop the stopwatch once it reaches steady state.
5
3
Figure A1: Location of inlet valves for step 3 and 5
6.5 General Shut-down Procedures
6.5.1. Switch off the pumps (P-101, P-102 and P-103), conductivity meter (QT-101)
and stirrer (M-101).
6.5.2. Switch off the heaters (HTR-101 and HTR-102) if they are on.
6.5.3. Switch off the power supply at the control panel.
6.5.4. Close FM-101.
6.5.5. Open valves V-102 and V-104 to drain all the solutions from feed tanks T-101
and T-102. Otherwise, close valves V-102 and V-104 to keep the solutions for
subsequent experiment.
6.5.6. Open V-105 to drain any solution from the reactor R-101 and store any
solution needed in a proper labelled container. Consult the lab manager regarding
chemical storage.
6.5.7. Open valve V-106 to drain any solution from the product tank T-103.
6.5.8. Properly dispose of any unwanted material, consult the lab manager for
guidance.
6.5.9. Fill up the reactor tank with clean water till 1/2 full to protect the temperature
6.5.10. Close all the valves except V-107.
36
7.0 RESULT
7.2 Plot calibration curve graph. (Conductivity vs. conversion; concentration of NaOH
vs. conversion).
7.3 Plot a graph of conversion vs. time.
7.4 For an equimolar reaction with the same initial reactants‟ concentration (CA0 = CB0),
the rate law is shown to be:
where CA is the concentration of NaOH in the reactor at time t. Plot a graph of “ln
(-dCA/dt)” vs. “ln (CA)”and evaluate the slope and y-axis intercept.
7.5 Determine the order of the reaction, α and the rate constant, k from the slope and
intercept values.
8.0 DISCUSSION
8.1 Discuss the reaction rate constant and reaction order in batch reactor.
9.0 CONCLUSION
37
APPENDIX B3: Sample Table for Preparation of Calibration Curve
Solution Mixtures
Concentration Conductivity
Conversion 0.1 M
0.1 M NaOH H2O of NaOH (M) (mS/cm)
Na(Ac)
0% 100 mL
25% 100 mL
50% 100 mL
75% 100 mL
100% 100 mL
38
APPENDIX C3: Sample table for experimental data
Conductivity
Time (s)
(mS/cm)
10
20
30
40
50
60
70
80
90
100
39
EXPERIMENT 5
Effect of Temperature on Reaction and Reaction’s Activation Energy
for Batch Reactor
1.0 OBJECTIVES
1.1 To observe and control the operation of a batch reactor for saponification reaction
between Sodium Hydroxide and Ethyl Acetate.
1.2 To determine the effect of temperature on the extent of conversion.
1.3 To determine the value of the reaction’s activation energy.
CO2: Ability to ANALYZE and solve various problem related to reactor design and reaction
process.
3.0 INTRODUCTION
In the majority of industrial chemical processes, reactor is the key equipment in which raw
of chemical reactors is thus crucial to the whole success of an industrial process. Reactors
can take a widely varying form, depending on the nature of the feed materials and the
products. Understanding the behavior of how reactors function is necessary for the proper
design, control and handling of a reaction system. Two main types of reactors are batch
reactor and continuous flow reactor.
The Reactor Basic Unit (Batch Reactor) has been designed for students‟ experiments on
chemical reactions in liquid phase under isothermal and adiabatic conditions. The unit
comes complete with a glass reactor, constant temperature water circulating unit,
temperature and conductivity measurements. Student shall be able to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide.
40
4.1 THEORY
4.2 Rate of Reaction and Rate Law.
The rate at which a given chemical reaction proceeds can be expressed in several ways. It
can be expressed either as the rate of disappearance of the reactants, or the rate of
formation of products. In the following reaction,
aA + bB cC + dD [1-1]
A and B are the reactants, while C and D are the products. a,b,c,d are the stoichiometric
coefficients for the respective species.If species A is considered as the reaction basis, then
the rate of reaction can be represented by the rate of disappearance of A. It is denoted by
the symbol –rA . The numerical value of the rate of reaction, –rA is defined as the number of
moles of A reacting (disappearing) per unit time per unit volume, and has the typical unit of
mol/dm3.s. Similarly, the rate of reaction can also be represented by the rate of
disappearance of another species, such as –rB and the rate of formation of a product, such
as rC or rD . They can be related in the following equation,
 rA r rC rD
B
a  b  c  d
[1-2]
4.3 Conversion
Using the reaction shown in Equation [1-1], and taking species A as the basis of calculation,
the reaction expression can be divided through by the stoichiometric coefficient of species A,
in order to arrange the reaction expression in the form,
b c d
A+ B  C + D [2-1]
a a a
The expression has now put every quantity on a „per mole of A‟ basis.
A convenient way to quantify how far the reaction has progressed, or how many moles of
products are formed for every mole of A consumed; is to define a parameter called
conversion. The conversion XA is the number of moles of A that have reacted per mole of A
fed to the system,
moles of A reacted
X A  [2-2]
moles of A fed
41
Because the conversion is defined with respect to the basis of calculation (species A), the
subscript A can be eliminated for the sake of brevity and let X = XA .

To perform a mole balance on any system, the system boundaries must first be specified.
The volume enclosed by these boundaries will be referred to as the system volume. In
this example, a mole balance will be performed on species j in a system volume, where
species j represents the particular chemical species of interest.
Fj0 Fj
A mole balance on species j at any instant in time, t, yields the following equation,
Rate of j Rate of j  Rate of j   Rate of j 

into   out of   produced   accumulated 
    
system  system  within system within system
       
volume  volume   volume   volume 

dNj
Fj0 – Fj + Gj = [3-1]
dt
where Nj represents the number of moles of species j in the system at time t.
42
Figure 2: Unit construction for Batch reactor
43
Table 1: List of valves.

Description
Tag Location
V-105 Drain valve of R-101
V-106 Drain valve from T-103
V-107 Discharge Valve from T-104 to Heating Coil
Height : 1.50 m
Overall Dimension
Width : 1.10 m
Depth : 0.80 m
General Working Area : Ventilated, approximately 10m2

Requirement
Chemical : Ethyl Acetate & Caustic Soda (0.1M)
are suggested
Utility : 1. Electrical supply: 230VAC, 1-

phase, 50Hz
2. Water: Laboratory main supply with
drainage
44
The Reactor Basic Unit (Batch), Model: K1051)

includes the following items:
Specifications
a) Bench
A bench constructed from aluminium frame and
chemically resistant worktop, comes with lockable
castor wheels.
b) Reactor (R-101)
Reactor Vessel : Borosilicate glass; top and bottom
plate made of non-corroding material
Reactor Volume : 5 liters
Heating System : Heating Coil
Ports : Feed inlets, temperature transmitter,
conductivity, drainage
c) Stirrer System (M-101)

Variable Speed : 50 to 2200rpm; with speed
controller and indicator
Impellers : 50mm diameter, stainless steel
Electrical : 240VAC/1-phase/50-60Hz/50W
d) Feed Tanks (T-101, T-102)

e) Product Tank (T-103)

45
f) Hot Water Tank (T-104)

g) Feed Pumps (P-101, P-102)

Type : Peristaltic
Capacity : 1 L/min
h) Water Feed Pump (P-103)

Type : Centrifugal
Max Pressure Head : 15m
i) Flow Control (FI-101)

Type : Rotameter
Control valve : Needle valve
Range : 0.5 - 4LPM
j) Conductivity Meter (QT-101)

Sensor range : 0 to 200 mS/cm
Output : 4 to 20 mA
k) Temperature Transmitter
(TT-101, TT-103 & TT-104)
Type : RTD, Pt100
Range : 0 - 100 °C
l) Control Panel
All necessary electrical components and data
acquisition modules are housed in the control panel.
Instrumentations and digital displays are panel
mounted.
46
6.1 PROCEDURES
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O
6.2.2 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.
0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL
Na(Ac)
100% conversion : 100 mL Na(Ac)
6.3 General Start-up Procedures
6.3.1. Perform a quick inspection to make sure that the equipment is in proper
working condition.
6.3.2. Ensure that all valves are initially closed and all power supply switch are turn
off.
6.3.3. Switch on the main power and power switch on the control panel.
6.3.4. Open valves V-101 and V-103.
6.3.5. The equipment is now ready to use.
6.4 Experimental Procedures

6.4.1 Saponification at room temperature (approx. 28°C)
1) Prepare 8L of 0.1M NaOH and Et(Ac) solution into respective feed tank T-101
and T-102.
2) Switch on the pump P-101 to charge 1L of NaOH into the reactor tank.
3) Switch off the pump P-101 and close the inlet valve and then switch on
conductivity meter (QT-101) on the control panel.
4) Switch on pump P-102 to charge 1L of Et(Ac) into the reactor tank, which make
up a total 2L of solution in the reactor.
5) Switch off the pump P-102 and close the inlet valve.
6) Switch on stirrer (M-101) on the control panel. Set the stirrer speed to
47
approximately 500 rpm.
7) Record the initial conductivity value (QI-101).
8) Start the stopwatch immediately.
9) Start monitoring and record the conductivity value (QI-101) in Table A2.2 for
every 10 seconds.
10) Stop the stopwatch once it reaches steady state.
6.4.2 Saponification at 40°C & 50°C

1. Set the TT-101 controller on the control panel to 40°C.
2. Switch on heater HTR-101 to heat up the NaOH solution in T-101 to temperature

of 40°C.
3. Switch on pump P-102 to charge 2L of Et(Ac) in R-101. Then switch off pump P-
102 and close the inlet valve (refer to Figure A2).
4. Switch on heater HTR-104 to heat up the water in T-104 to temperature of 45°C.
5. Switch on P-103 to circulate the hot water in the heating coil.
6. Adjust the needle valve on the rotameter to a flow rate of 4LPM.
7. Observe the reading of TT-103 on the control panel which indicates the
temperature of solution in R-101.
8. Switch on stirrer M-101 to provide a uniform heating for solution.
9. Switch off heaters HTR-101 and HTR-104 once the temperatures TT-101 and TT-
103 achieve 40°C.
10. Switch off stirrer M-101.
11. Switch on the pump P-101 to charge 2L of NaOH into the reactor R-101. Then,
switch off P-101 and close the inlet valve (refer to Figure A2).
12. Switch on the conductivity meter (QT-101) and stirrer (M-101) on the control
panel. Set the stirrer speed to approximately 500 rpm.
13. Record the initial conductivity value and start the stopwatch immediately.
14. Start monitoring and record the conductivity value (QI-101) in Table APPENDIX
C4 for every 10 seconds.
15. Stop the stopwatch once it reaches steady state.
16. Repeat the experiment for reaction at 50°C by setting the temperature according
to the set temperature below:
Temperature Controller TT-101 TT-104
Set Temperature (°C) 50 55
48
11
3 1
Figure A2: Location of inlet valves for step 3 and 11
6.5 General Shut-down Procedures
6.5.1. Switch off the pumps (P-101, P-102 and P-103), conductivity meter (QT-101)
and stirrer (M-101).
6.5.2. Switch off the heaters (HTR-101 and HTR-102) if they are on.
6.5.3. Switch off the power supply at the control panel.
6.5.4. Close FM-101.
6.5.5. Open valves V-102 and V-104 to drain all the solutions from feed tanks T-101
and T-102. Otherwise, close valves V-102 and V-104 to keep the solutions for
subsequent experiment.
6.5.6. Open V-105 to drain any solution from the reactor R-101 and store any
solution needed in a proper labelled container. Consult the lab manager regarding
chemical storage.
6.5.7. Open valve V-106 to drain any solution from the product tank T-103.
6.5.8. Properly dispose of any unwanted material, consult the lab manager for
guidance.
6.5.9. Fill up the reactor tank with clean water till 1/2 full to protect the temperature
6.5.10. Close all the valves except V-107.
49
7.0 RESULT
7.2 For a second order reaction, the rate law is shown to be:
Integrating with CA=CAO at t=0
Rearranging
where CA0 is the initial concentration of reactant NaOH in the reactor. For each
temperature value, plot the graph of “1/CA” vs. time, t and evaluate the slope and y-
axis intercept.
7.3 Determine the rate constant, k from the slope value for different temperature
values. Examine the change in the rate constant.
7.4 Plot a graph of “ln k” vs. “1/T” and evaluate the slope and y-axis intercept.
7.5 Calculate the saponification reaction’s activation energy, E and Arrhenius constant,
A from the slope and intercept values using the Arrhenius equation.
E
k(T ) Ae E / RT or ln k ln A  (1/ T )
R
where E = activation energy [J/mol]

A = Arrhenius constant
R = universal gas constant = 8.314 J/mol.K
T = absolute temperature [K]
8.0 DISCUSSION
8.1 Discuss the effect of temperature on reaction and reaction’s activation energy for
batch reactor.
9.0 CONCLUSION
50
Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL
25% 100 mL
50% 100 mL
75% 100 mL
100% 100 mL
51
APPENDIX C4: Sample table for experimental data
Conductivity
Time (s)
(mS/cm)
10
20
30
40
50
60
70
80
90
100
52
EXPERIMENT 6
Effect of Residence Time on the Reaction in Catalytic Tubular
Reactor
1.0 OBJECTIVES
1.1 To carry out a hydrolysis reaction of Et(AC) in a catalytic packed bed reactor.
1.2 To determine the effect of residence time on the conversion in catalytic packed bed
reactor.
CO3: Ability to EVALUATE the catalytic reaction mechanism and Residence Time
Distribution (RTD) functions in reactors.
3.0 INTRODUCTION
In the majority of industrial chemical processes, the reactor is the key equipment in which
raw materials undergo a chemical change to form desired products. The design and
operation of chemical reactors is thus crucial to the whole success of an industrial process.
Reactors can take a widely varying form, depending on the nature of the feed materials and
the products. Understanding the behaviour of how reactors function is necessary for the
proper control and handling of a reaction system. Basically, there are two main groups of
reactors, batch reactors and continuous flow reactors.
The SOLTEQ® Catalytic Packed Reactor (Model: BP 105) has been designed for
students’ experiments on chemical reactions in liquid phase under isothermal and adiabatic
conditions. The unit comes complete with a jacketed tubular reactor, reactant feed tanks
and pumps, temperature sensors and conductivity measuring sensors. The reactor will
enable students to conduct the acid-catalysed liquid-phase hydrolysis of ethyl acetate
(EtAC) to ethanol (EtOH) and acetic acid (HAc), using an immobilized anion ion-exchange
resin (Amberlyst 15 (dry)) as catalyst:
CH3COOC2H5 + H2O = CH3COOH + C2H5OH
Figure 1 illustrates the process flow diagram for the catalytic packed flow reactor unit.
53
Figure 1: Process flow diagram for the catalytic packed bed reactor unit.
4.0 THEORY
4.1 Rate of Reaction and Rate Law

The rate at which a given chemical reaction proceeds can be expressed in several
ways. It can be expressed either as the rate of disappearance of the reactants, or the
rate of formation of products.
Let the reaction be:
A  B + D, rate = kC (1)
A = ethyl acetate (EtAC), B = acetic acid (HAc), D = ethanol (EtOH). Let C be the
EtAC concentration, V be the running volume (neglect the volume occupied by
catalyst) of a plug flow reactor of total volume, VF, and Q be volumetric flow rate.
Assuming first order reaction, the steady state reactor equation is:
dC/dV = -(1/Q)kC, C(0) = C0 (2)

for 0 <= V <=VF
54
And with k the reaction rate constant, assumed to be a function of temperature only.
Integrating the above equation:
C(VF) = C0exp(-kVF/Q) (3)
From stoichiometry, we have:
CF = C(VF) = C0 - CB (4)
Where CB is the effluent concentration of acetic acid (mol/L). and C0 is the feed
concentration.
From the integrated equation:
kVF = ln(C0/CF) or k = (Q/VF)ln(C0/CF) (5)
where k(T) = b1exp(-E/RT) which follows Arrhenius equation

where E = activation energy, R = gas constant, b1 = parameter
If a plot of ln(k) vs 1/T is drawn, a straight line with slope –E/R will be get.
4.2 Conversion
Using the reaction shown in Equation (1), and taking species A as the basis of
calculation, the reaction expression can be divided through by the stoichiometric
coefficient of species A, in order to arrange the reaction expression in the form,
b d
A+ B+ D (6)
a a
The expression has now put every quantity on a ‘per mole of A’ basis.
A convenient way to quantify how far the reaction has progressed, or how many
moles of products are formed for every mole of A consumed; is to define a parameter
called conversion. The conversion XA is the number of moles of A that have reacted
per mole of A fed to the system,
moles of A reacted
XA  (7)
moles of A fed
Because the conversion is defined with respect to the basis of calculation (species
A), the subscript A can be eliminated for the sake of brevity and let X = XA .

To perform a mole balance on any system, the system boundaries must first be
specified. The volume enclosed by these boundaries will be referred to as the
system volume. In this example, a mole balance will be performed on species j in a
system volume, where species j represents the particular chemical species of
interest.
Fj0 Fj
Gj
55
A mole balance on species j at any instant in time t, yields the following equation,
Rate of flow  Rate of flow  Rate of generation of j  Rate of j 

 of j into   of j out of   by chemical reaction   accumulate d 
    
 system   system   within system   within system
       
 volume   volume   volume   volume 

dN j
Fj0 – Fj + Gj = (8)
dt
where Nj represents the number of moles of species j in the system at time t. If all the
system variables (e.g. temperature and concentration) are spatially uniform
throughout the system volume, the rate of generation of species j, Gj , is just the
product of the reaction volume, V and the rate of formation of species j, rj ,
Gj  r jV (9)
Suppose that the rate of formation of species j for the reaction varies with the position
in the system volume. Thus, the total rate of generation within the system volume is
the integral of all the rates of generation in each of the subvolumes,
V
Gj   r j dV (10)
Therefore, the general mole balance equation for any chemical species j that is
entering, leaving, reacting and/or accumulating within any system volume V, is,
V dN j
Fj 0  Fj   r j dV  (11)
dt
From this general mole balance equation, the design equations for various types of
industrial reactors such as batch, semibatch and continuous flow reactors can be
developed. Upon evaluation of these design equations, the time (batch) or reactor
volume (continuous) necessary to convert a specified amount of reactants to
products can then be determined.
4.4 Tubular Flow Reactors

The tubular flow reactor (TFR) (sometimes called plug flow reactor (PFR)) is also
commonly used in industry in addition to the CSTR and batch reactor. It consists of a
cylindrical pipe and is normally operated at steady state. For analysis purposes, the
flow in the system is considered to be highly turbulent and may be modeled by that of
plug flow. Thus, there is no radial variation in concentration along the pipe.
In the tubular reactor, the reactants are continually consumed as they flow down the
length of the reactor. In modeling the tubular reactor, the concentration is assumed to
vary continuously in the axial direction through the reactor. Consequently, the
reaction rate, which is a function of concentration for all but zero order reactions, will
56
also vary axially.
y Δy
FA0 FA
FA(y) FA(y + Δy)
ΔV
Figure 3: Tubular flow reactor (TFR)
To develop the TFR design equation, the reactor volume shall be divided into a
number of subvolumes so that within each subvolume ΔV, the reaction may be
considered spatially uniform. Assuming that the subvolume is located a distance y
from the entrance of the reactor, then FA(y) is the molar flow rate of A into volume ΔV
and FA(y + Δy) is the molar flow rate of A out of the volume. In a spatially uniform
subvolume ΔV,
V
 rA dV  rA V (12)
For a tubular reactor at steady state, the general mole balance is reduced to,
dN A
 0
dt
FA ( y )  FA ( y  y )  rA V  0 (13)
In the above expression, r A is an indirect function of y. That is, r A is a function of

reactant concentration, which is a function of the position, y down the reactor. The
volume, ΔV is the product of the cross-sectional area, A of the reactor and the reactor
length, Δy.
V  Ay (14)
Substituting Equation (13) into Equation (12) yields,
 F ( y  y )  FA ( y ) 
 A    ArA (15)
 y 
Taking the limit as Δy approaches zero,
 F ( y  y )  FA ( y )  dFA
lim  A
y   dy  ArA (16)
y 0
 
It is usually most convenient to have the reactor volume, V rather than the reactor
length, y as the independent variable. Accordingly, the variables ‘Ady’ can be
changed to dV to obtain this form of the design equation for a TFR,
57
dFA
 rA (17)
dV
Note that for a reactor in which the cross-sectional area, A varies along the length of
the reactor, the design equation remains unchanged. This means that the extent of
reaction in a plug flow reactor does not depend on its shape, but only on its total
volume.
If FA0 is the molar flow rate of species A fed to a system operated at steady state, the
molar flow rate at which species A is reacting within the entire system will be [FA0X].
The molar feed rate of A to the system minus the rate of reaction of A within the
system equals the molar flow rate of A leaving the system, FA . This is shown in
mathematical form to be,
FA  FA0  FA0 X  FA0 (1  X ) (18)
The entering molar flow rate FA0 is just the product of the entering concentration C A 0
and the entering volumetric flow rate v 0 ,
FA0  C A0v 0 (19)
Combining Equation [4-7] and Equation [4-6] yields the design equation with a
conversion term for the TFR,
dX
FA0   rA (20)
dV
Rearranging and integrating Equation 19 with the limit V = 0 when X = 0, we obtain

the plug-flow reactor volume necessary to achieve a specified conversion X,
X dX
V  FA0  (21)
0  rA
5.0 DESCRIPTION OF EQUIPMENTS
Before operating the unit and running experiments, students must familiarize themselves
with every components of the unit. Please refer to Figure 1 to understand the process.
Packed Reactor
Material : High quality borosilicate glass
Volume : approx. 0.6 L
Feed tanks
Cylindrical vessels made of stainless steel
Water de-ionizer fitted to Feed Tank 1 and Feed tank 2
Product tank
Tank made of stainless steel
Pre-heater
Cylindrical vessel made of stainless steel
58
Internal coils for reactants
Feed pumps
Type : Peristaltic Pump
Max. Speed : 100 rpm
Power : 230V/50Hz/1-phase
Instrumentations
Flow measurements from the Peristaltic Pump 1 & 2
Temperature measurements (TT1 to TT4)
Conductivity measurements (Q1, Q2)
5.1 VALVES AND INSTRUMENTS LIST
Valves list:
Tag Location
V1 Feed Tank 1 drain valve
V2 Reactants outlet valve from Feed Tank 1
V3 Feed Tank 2 drain valve
V4 Reactants outlet valve from Feed Tank 2
V5 Reactants inlet valve into Reactor
V6 Reactants drain valve from Reactor
V7 Water circulator inlet valve from Water Circulator
V8 Deionized water inlet valve into Feed Tank 2
V9 Deionized water inlet valve into Feed Tank 1
V10 Product drain valve from Product Tank
V11 Drain valve for water bath circulator
Instruments list:
Tag Description Units Range Accuracy
mS/c 0.0 –
Q1 Conductivity in ± 1% FS
m 20.00
mS/c 0.0 –
Q2 Conductivity out ± 1% FS
m 20.00
0.0 –
TT1 Reactor inlet temparature °C ± 0.5°C
200.0
0.0 –
TT2 Reactor outlet temparature °C ± 0.5°C
200.0
0.0 –
TT3 Circulator inlet temperature °C ± 0.5°C
200.0
0.0 –
TT4 Circulator outlet temperature °C ± 0.5°C
200.0
59
6.0 PROCEDURES
The reaction to be studied is the hydrolysis reaction of ethyl acetate Et(AC).
EtAC  EtOH + HAc
Since only acetic acid, HAc will conduct electricity, therefore the conductivity value
depends on HAc only.
a) 1 liter of HAc
b) 2 liter of deionized water
6.2.2 Prepare 200 mL HAc solution by adding 5 mL HAc into 195 mL deionized water.
Determine the conductivity of HAc solution at this concentration.
6.2.3 Repeat step 6.2.2 by changing the volume of HAc until 100 mL in the increment of
5mL into the deionized water.
6.2 General Start-Up procedures

6.2.1 Ensure that all valves are initially closed.
6.2.2 Prepare a 10 liter of ethyl acetate solution by adding 400mL of ethyl acetate
into 9.6 L of deionized water. And pour the solution into feed tank 1.
6.2.3 Fill in 10 L of deionized water into feed tank 2 by opening V8.
6.2.4 Turn on the power for the control panel.

6.2.5 The unit is now ready for experiment.
6.3 Experiment Procedures
6.3.1 Perform the general start-up procedures as in Section 6.1.
6.3.2 Open valves V2, V5, and V7.

6.3.3 Turn on Pump 1 and adjust the flowrate controller to give a constant flow rate of 15
mL/min by adjusting the speed (RPM) of Pump 1.
6.3.4 Allow Et(AC) solution to enter the catalytic packed bed reactor.
6.3.5 Start monitoring the inlet (Q1) and outlet (Q2) conductivity values until they do not
change over time. This is to ensure that the reactor has reached steady state.
(Note: This may take up to 1 hour to reach steady state.)
6.3.6 Record both inlet and outlet steady state conductivity values in table of Appendix C.
Find the concentration of HAc exiting the reactor and extent of conversion from the
60
calibration curve.
6.3.7 Before start the new experiment, turn off pump 1. Turn on pump 2 to flow in the
deionized water (150 mL/min) into the reactor until obtain a low conductivity value.
6.3.8 Repeat the experiment (steps 6.4.3 to 6.4.7) for different residence times by changing the
feed flow rates of EtAC to 20 and 25 mL/min.
6.4 General Shut-Down procedures

6.4.1 Switch off the pump.
6.4.2 Set the water circulator to room temperature.
6.4.3 Keep the water circulating through the reactor while the circulator motor is running to
allow the reactor to cool down to room temperature.
6.4.4 If the equipment is not going to be used for long period of time, drain all liquid from
the unit. Rinse the feed tanks and product tank with clean water.
6.4.5 Turn off the power for the control panel.
7.0 RESULT
7.1 Record all the results in the table (Appendix C) for every reading taken by
conductivity meter.
7.2 Plot a graph of conductivity vs. concentration of HAc.
7.3 Plot a graph of conversion vs. conductivity for calibration curve.
7.4 Plot a graph of conversion vs. residence time. The reactor’s residence time is
defined as the reactor volume (VTFR=0.387 L) divided by the total feed flow rates.
Residence time,
VTFR

v0
8.0 DISCUSSION
8.1 Discuss the effect of residence time on conversion.
9.1 CONCLUSION
61
APPENDIX A5: Physical Properties of Ethyl Acetate and Acetic Acid.
Property Ethyl Acetate Acetic Acid
Formula CH3COOCH2CH3 CH3COOH
Appearance Clear liquid Clear liquid
Normal boiling point 77.1°C 118.1°C
Normal melting point -84.0°C 16.5°C
Density 0.897 g/mL @ 25°C 1.049 g/mL @ 25oC
Refractive index 1.3274 @ 20°C 1.3716 @ 20°C
Volume of HAc Concentration Conductivity

(mL) of HAc (mol/L) (mS/cm)
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
62
APPENDIX C: Sample Tables for experiment
Time (min) Outlet Conductivity, Q2 (mS/cm)
15 mL/min 20 mL/min 25 mL/min
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
Inlet Outlet Exit concentration of

Flow rate of Residence time, Conductivity, Q2 HAc (mol/liter) Conversion,
Conductivity, Q1
EtAC (mL/min) τ (min) (mS/cm) X (%)
(mS/cm)
15
20
25
Concentration of Et(AC) in feed vessel, CAO= _____ mol/L
63
EXPERIMENT 7
Effect of Pulse Change in Input Concentration to the
Concentration of solute in Continuous Stirred Tank Reactor
(CSTR) in Series.
1.0 OBJECTIVES
1.1 To observe and control the operation of a CSTR in series.

1.2 To observe the effect of pulse change in input concentration to the concentration of
solute.
1.3 To determine the mean residence time, variance, and skewness for the residence
time distribution of CSTR in series.
CO3: Ability to EVALUATE the catalytic reaction mechanism and Residence Time
Distribution (RTD) functions in reactors.
3.0 INTRODUCTION
In the majority of industrial chemical processes, a reactor is the equipment in which raw
of chemical reactors is thus crucial to the whole success of the industrial operation.
Reactors can take a widely varying form, depending on the nature of the feed materials and
the products. One particular type of process equipment is the continuous stirred tank
reactor. In this reactor, it is important to determine the system response to a change in
concentration. This response of concentration versus time is an indication of the ideality of
the system.
The SOLTEQ® CSTR In Series (Model: BP 107A, Figure 1 and 2) has been designed to
demonstrate the dynamics of the simplest classic case of a well-mixed, multi-staged
process operation. The unit comes with three stirred tank reactors connected in series
complete with sump tanks and pumps. Instruments are provided for the measurement of
conductivity in each reactor. Students may select either step change input or pulse input to
the reactor and will continuously monitor the responses in each reactor at a suitable
interval. Based on the experimental data, students will be able to determine the mean
residence time (tm), the variance (σ2), and the skewness (s 3) of the residence time
distribution (RTD) function.
64
5
1
3 7
8
Figure 1: Unit Assembly of CSTR in Series (Model: BP107A)
1. Stirrers 5. Conductivity Indicator

2. Conductivity Sensor 6. Temperature Indicator
3. Reactors 7. Peristaltic Pump 1
4. Sump Tank 8. Peristaltic Pump 2
65
Figure 2: Process Diagram for CSTR Dynamics (BP 107A)
4.0 THEORY
4.1 Tracer Analysis on the Transient Behaviour of Continuous Stirred-Tank in Series
The tracer analysis will help us understand the transient behaviour of the continuous
stirred tank reactor in series by injecting an inert chemical (e.g. salt) into the reactor
at time t = 0. The most common methods of injection are step input or pulse input.
The conductivity measurement will indicate the progression of the tracer throughout
the stirred tank in series (Figure 3).
Figure 3: Stirred tanks in series

66
The residence time distribution (RTD) function is determined from the E(t) curve.
For step input, E(t) is defined as:

d  C (t ) 
E (t )   
dt  C0 
Using pulse injection tracer, E(t) is defined as:
C (t )
E (t )  
 0
C (t )dt
The space time or average residence time  is defined as being equal to V/v and always equal
to the mean residence time, tm which is the first moment of the RTD function.

tm  0
tE (t )dt
The second and third moments of the RTD functions are variance (  2 ) and skewness
( S3 ), respectively.

 2   (t  tm )2 E (t )dt
0
1 
S3 
 32  0
(t  tm )2 E (t )dt
For equal-size tank in series, the RTD function for CSTRs n in series can be
generalized as:
t n1e t  i
E (t ) 
(n  1)! in
where  i   n , and  represents the total reactor volume divided by the flow rate (
  tm ).
For three reactors in series, it can be shown that the tracer concentration in the effluent
from the third reactor is
C0 t 2  t /  i
C3  2 e
2 i
And the RTD function is
67
2
C3 (t ) t t / i
E (t )   e

2 i3

0
C3 (t )dt
Figure 4: Tank in series model
5.0 DESCRIPTION OF EQUIPMENTS
Before operating the unit and running experiments, students must familiarize themselves
with every components of the unit. Please refer to Figure 2 to understand the process.
Reactors (R1, R2, R3)

1-L reactors made of borosilicate glass
Variable speed stirrer for each reactor
Conductivity sensor for each reactor
Gravity flow between reactors
rd
Adjustable overflow tube at 2nd and 3 reactors
Stirrers (M1, M2, M3)

Variable speed: 50 – 2000 rpm with LCD display
Max. torque: 30 Ncm
Power: 230VAC/50-60Hz/70W
Stainless steel shaft and impeller
Feed tanks (B1, B2)

30-L cylindrical vessel made of stainless steel Water
de-ionizer fitted to tank B1
Feed pumps (P1, P2)

Peristaltic pumps Max delivery rate: 0-300RPM
Power: 230VAC / 50 Hz
Dead time coil (R4)

Material: 3/8” stainless steel tubing Volume: approx. 200 ml
68
Instrumentations
Conductivity (QT01, QT02, QT03, QT04):
Range : 0 to 200 mS/cm
Output : 4 to 20 mA
Display : LED display for conductivity controller with digital display for each
sensor mounted on the control panel
Temperature Sensor ( TT01, TT02, TT03)

Range: 0-100 °C
5.1 VALVES AND INSTRUMENTS LIST
Table 1: Valve configuration
Tag Location Initial position

V1 Inlet valve for pump P1 Close
V2 Drain valve for feed tank B1 Close
V3 Inlet valve for deionized water Close
V4 Inlet valve for pump P2 Close
V5 Drain valve for feed tank B2 Close
V6 Three way valve Close
V7 Drain valve for waste tank Close
V8 Inlet valve for reactor R1 Close
V9 Inlet valve for reactor R3 Close
V10 Inlet valve for dead time coil Close
V11 By-pass valve from reactor R1 to reactor R2 Close
V12 Drain valve for reactor R1 Close
V15 By-pass valve from reactor R2 to reactor R3 Close
V16 Drain or sampling valve for reactor R3 Close
V18 Drain for deionized water Close
V19 Vent valve Open
V20 Vent valve Open
V21 Vent valve Open
Table 2: Instrumentation list
Tag Description Units Range Accuracy

QT01 Conductivity mS/cm 0.0 – 200.0 ± 1% FS
TT01 Temperature oC 0 – 100 ± 1%
69
6.0 PROCEDURES
6.1 General Start-Up procedures

6.1.1 Ensure all the valves are closed.
6.1.2 Prepare a 30-L of salt solution (e.g. sodium chloride, NaCl; 0.025 M).
6.1.3 Fill the feed tank B2 with the NaCl solution.
6.1.4 Turn on the power for the control panel.
6.1.5 Fill up feed tank B1 with de-ionized water.
6.1.6 Open valve V1, V8, V11 and V15. Turn the three-way valve V6 handle
pointing toward yourself. Switch on pump P1 and regulate the pump speed to
obtain a flow rate of approximately 190 ml/min (40 RPM). Switch off pump P1.
6.1.7 Open valve V4. Turn the three-way valve V6 handle to the right side. Switch
on pump P2 and regulate the pump speed to obtain flow rate of approximately
190 ml/min (40 RPM). Switch off pump P2.
6.1.8 Switch on pump P1. Allow the deionized water to overflow from reactor R3
until the conductivity value stabilizes at low value. Switch off pump P1.
6.1.9 The unit is now ready for experiments.
Note: Please make sure the vent valves at the top of the 3 reactors are
always open. Unless there are air traps inside the by-pass tubing
(from reactor 1 to 2 and from reactor 2 to 3)
To eliminate the air trap, close the vent valve and pump in the
water, when the water flows out from the second reactor, open the
vent valve.
Please ensure that there are no bubbles traps inside the probe
QT01 until QT03 as it will affect the results taken.
6.2 Experiment Procedures

6.2.1 Perform the general startup as describe in section 6.1.
6.2.2 Ensure the feed tank B1 is filled with deionised water.
6.2.3 Ensure that feed tank, B2 is filled with 30-L of 0.025M sodium chloride
solution.
6.2.4 Set the 3-way valve V6 handle pointing to yourself.
6.2.5 Open valve V8, V11, and V15. Switch on Pump P1 to initially fill up all three
reactors with deionised water.
6.2.6 Regulate the pump speed to 40 RPM to obtain a flow rate of approximately
190 ml/min. Make sure that no air bubbles are trapped in the piping.
Note: It is important to maintain the liquid level in each reactor. Adjust the
flowrate if necessary.
6.2.7 Switch on stirrers 1, 2 and 3. Set the stirrer speed to approximately 200 rpm.
6.2.8 Continue pumping the de-ionized water until all conductivity readings (QT01,
QT02, QT03) are stable at low values.
6.2.9 Record these conductivity values at time t0.
6.2.10 Switch off pump P1. Quickly set the 3-way valve V6 handle to the right side.
70
Switch on pump P2 and start the timer simultaneously.
6.2.11 Let the pump P2 operate for 2 minutes, and then switch off pump P2. Quickly
switch the 3-way valve V6 handle pointing to yourself. Switch on pump P1 and
let it run till the end of experiment.
6.2.12 Record all conductivity values (QT01, QT02, QT03) at 1 minute interval in an
appropriate table.
6.2.13 Continue recording the conductivity values until all readings are almost
constant.
6.2.14 Switch off pump P1 and all the stirrers, M1, M2 and M3.
6.2.15 Drain all liquids in each reactor by opening valves V11 until V18.
6.3 General Shut-Down procedures
6.3.1 Switch off both pumps P1, P2. Close valves V1 and V4.
6.3.2 Open valves V12 to V17 to drain all liquid into the waste tank.
6.3.3 Make sure that the reactor and tubings are cleaned properly by flushing the
system with de-ionized water until no traces of chemical are detected.
6.3.4 If the equipment is not going to be used for a long period of time, drain all
liquid from both feed tanks by opening valves V2 and V5. Rinse the feed tanks
with clean water.
6.3.5 Turn off the power for the control panel.
7.0 RESULT
7.1 Record all the results in the table (Appendix A6) for every reading taken by
conductivity meters.
7.2 Plot a graph of all the all conductivity values (QT01, QT02, QT03) vs. time.

7.3 Calculate the value of the integral  C (t )dt
0
. Use any suitable numerical method. Do
not include integral below the stable low level value.

7.4 Calculate the values of E(t).
C (t )
E (t )  
 C (t )dt
0
7.5 Plot E(t) as a function of time. This is the residence time distribution (RTD)
for the particular CSTR.
7.6 Calculate the following:
a) Mean residence time,

tm   tE (t )dt
0
b) Second moment, variance,
71

 2   (t  tm )2 E (t )dt
0
c) Third moment, skewness,


1
S   (t  t
3
)3 E (t )dt
32 0
m
8.0 DISCUSSION
8.1 Discuss the transient behavior in the three CSTRs in series.
9.2 CONCLUSION
72
APPENDIX A6: Sample Tables for experiment
Time (min) Q1 (mS/cm) Q2 (mS/cm) Q3 (mS/cm)
73

(KMK20303) Lab Module Sem 1 20232024

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

(KMK20303) Lab Module Sem 1 20232024

Uploaded by

Copyright:

Available Formats

LABORATORY

En. Zulkarnain Bin Mohamed

Faculty of Chemical Engineering

University Malaysia Perlis

CLEANLINESS AND SAFETY iii

EXPERIMENT 1 : INTRODUCTION TO THE LABORATORY SAFETY 1

EXPERIMENT 2 : EFFECT OF FLOW RATE ON THE REACTION 1

EXPERIMENT 3 : EFFECTS OF FLOW RATE AND REACTION 8

EXPERIMENT 4 : DETERMINATION OF REACTION RATE 15

EXPERIMENT 5 : EFFECT OF TEMPERATURE ON REACTION 27

EXPERIMENT 6 : EFFECT OF RESIDENCE TIME ON 40

EXPERIMENT 7 : EFFECT OF PULSE CHANGE IN INPUT 51

The Reaction Engineering Laboratory contains equipment that uses water or

 removal of spilled water (or any liquid) or chemicals

FOOTWARE – Wear fully covered shoes with strong grip.

EYE PROTECTION – Goggles must be used whenever necessary especially when

INSTRUCTION SHEETS – Any appropriate instruction sheets should be studied

There should be NO EATING in the laboratory. Smoking is strictly prohibited in all

In case of emergency, report to the Instructor in charge or

Hospital Tuanku Fauziah, Kangar 04-9763333

1.1 To identify applicable safety measures in performing the reaction engineering

2.0 COURSE OUTCOME

3.0 INTRODUCTION TO LABORATORY SAFETY

FOOTWARE – Wear fully covered shoes with strong grip.

INSTRUCTION SHEETS / LAB PROCEDURES – Any appropriate instruction sheets or lab

3.1 REACTOR ENGINEERING LEARNING APPARATUS

The apparatus for the reaction engineering laboratory is listed as follows:

4.0 EXPERIMENTAL PROCEDURES

1. Locate each reaction engineering apparatus provided in the laboratory.

5.1 RESULTS AND DISCUSSIONS

1. Write the general lab procedures in Reaction Engineering Lab

Conclude your findings related to importance of laboratory safety.

EFFECT OF FLOW RATE ON THE REACTION IN A CSTR

2.0 CORRESPONDING COURSE OUTCOME

From the general mole balance equation on a CSTR (Figure 1),

So, the design equations for the continuous-stirred tank reactor.

Figure 1: Mole balance on a CSTR

5.0 MATERIALS AND EQUIPMENT

5.1 Description of Apparatus

5.2 Description and Assembly

Figure 2: CSTR reactor-Front view.

Figure 3: CSTR reactor-Back view.

d. Feed Tank (T-101, T-102)

e. Product Tank (T-103)

f. Feed Pump (P-101, P-102)

g. Conductivity Meter (AT-101)

h. Temperature Transmitter (TT-101)

6.1 Preparation of Calibration Curve for Conversion vs Conductivity.

b. Mix the solutions according to Table 2 as shown.

1. Switch on the main power supply.

6.3 Experiment Effect of Flow Rate On The Reaction In A CSTR

6.4 Shut Down

1. Adjust the pumps speed to 260rpm.

5. Click “EXIT” on the pop out dialogue.

6. Switch off the power supply at the control panel.

APPENDIX A1: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C