Sultanate of Oman

University of Technology and Applied Sciences

Higher College of Technology

Chemical Reaction Engineering Practical (CHEE3203P)

Semester 2 Academic Year 2021-2022
Laboratory Manual Department Stamp
ENGINEERING DEPARTMENT

Student Name ID #
Section # 3,4 Day/Time
Name of Faculty Office Hours: Sunday 10am - 12pm
(Laboratory):
[email protected] 3 Last 13/02/22
E-mail Address: m Version No. Date of
Revision
Name of Course Mrs. Al Zaharaa Al Hinaai
Coordinator
Signature Date
(Lecturer):

Name of Faculty BUTHAINA HAMOOD ALI

Signature Date
Head (Lab): AL AISARI
Approved by: Specialization
Program
Coordinator’s Signature Date
Name:
Verified by: Section CAE EEE MIE
Curriculum
Committee Signature Date
Member:

CHEE3203P Reaction Engineering Practical Page 1

 CONTENTS

No. Activity Page No

1 Lab Safety 3
2 Equipment Description 5
3 Theoretical Principles 8
4 Experiment 1: Chemical Reagent Preparation 9
5 Experiment 2: Finding Reaction Rate 12
6 Experiment 3: Finding the activation energy 14
7 Experiment 4: The initial rate method 16

CHEE3203P Reaction Engineering Practical Page 2

 Chemical Engineering Laboratory

Basic Summary of Lab safety Watch 'Lab Safety' | Microsoft Stream

The Following is a list of basic, safe laboratory practices, which are expected of all
students. Many of these are common sense rules.

1. NO food and drinks are allowed in the laboratory at all time.

2. NO smoking in the laboratory.
3. NO horseplay in the laboratory.
4. NO Open sandals. Only covered shoes are to be worn in the laboratory.
5. NO jewellery during laboratory classes / workshop practical.
6. NO short sleeves. Legs must be covered with long pants.
7. NO bags, books and other personal items in the working area.
8. Must tie long hair back to reduce fire or chemical hazards.
9. Must wear the appropriate personal protective equipment during the experiment.
10. Must report all injuries, accidents and broken equipment immediately inform your
supervisor.
11. Must obtain a permission to work in the laboratory / workshop by laboratory
instructor.
12. Must be familiarize with the safety equipment (safety shower, emergency
eyewash, fire blanket, and fire extinguisher) in the laboratory and emergency
escape routes.

Preparation for Lab Work Watch 'Lab Instructions' | Microsoft Stream

1. Important Inspection

 Know the location and operation of the following:

 Fire Extinguishers
 Safety showers and Eye Wash Stations
 Fire Alarm Boxes
 Exit Doors
 Telephones

2. Preparing for Experiment

 Prepare for the experiment by reading all of the directions before you start the
lab. Be sure you understand all directions. Discuss the procedures with your lab
partner or team. Assign specific tasks to individuals, especially if time is a factor in
the procedure.

CHEE3203P Reaction Engineering Practical Page 3

  Before you begin work, make sure that you know how to operate the equipment
that will be used in the experiment.
 After you have completed your work, turn off all equipment and clean your work
area. Return all equipment and materials to the place that you got them. Report
any broken or missing equipment.
 Keep hands away from your face, eyes, mouth and body while using chemicals or
preserved specimens. Wash your hands before and after each experiment.
 Perform only those experiments authorized by your teacher. Never do an
experiment that is not called for in the laboratory procedures or your instructor.
 Do not work alone in the lab. When entering the room, do not touch any
equipment, chemicals or other materials in the laboratory area until you are
instructed to do so.
 Experiments must be personally monitored at all times. You will be assigned a
laboratory station at which to work. Do not wander around the room, distract
other students, or interfere with the laboratory experiments of others.

3. Material Safety Data Sheet (MSDS)

• Make sure every newly received chemical is accompanied with MSDS and the
MSDS should be kept in a designated file dedicated for MSDS only.
• Staff and students should familiarise themselves with MSDS and the location of
MSDS.
• For any incident involving chemicals that requires medical assistance, make
sure to present the MSDS to the medical personnel and return the MSDS in the
MSDS file.

CHEE3203P Reaction Engineering Practical Page 4

Equipment Description

Watch 'Equipment Description' | Microsoft Stream

The Armfield CEXC family is a range of chemical reactors specifically developed for the
teaching and demonstration of chemical reactor capabilities to chemical engineering
students. Real chemical reactions take place within the reactors, and Armfield have
developed a number of representative reactions which are easy and safe for students to use
in the laboratory environment. This range of small-scale chemical reactors comprises five
units, which represent the types of reactors found in the industry. Three of the reactors
mount on a common bench top service unit (CEXC) whilst the other two are free-standing.
PC based educational software is included along with the necessary interface device to
provide computer control, automatic logging of data and analysis of results. Reactors
comprise: Plug Flow, Laminar Flow, Stirred Tank, Tubular and Batch reactors.

The CEXC Chemical Reactors Teaching Unit provides the services required to run the
various reactor types. It includes a hot water re-circulator used to control the temperature
of the reactions, glass feed vessels for the reactants, two peristaltic pumps to pump the
reagents to the reactors, computer software for data logging, sensors and
instrumentation.
The CEXC is fully computer controlled, and supplied with software to allow the user to vary
the feed pump speeds and flow rates, to vary the heater power in the hot water, to
implement a PID control loop ensuring stable temperatures, switch on and off the hot
water pump, and to control the speed of the stirrers used on some of the reactors.

CHEE3203P Reaction Engineering Practical Page 5

Instrumentation for temperature and conductivity measurements is also supplied and
these values are displayed on the computer screen. Two ‘K’ type thermocouples are
included, one for the hot water and one for the reactor contents.
Note: An input for a third user supplied sensor is also provided for project work.
A dual-range conductivity sensor allows for a wide range of operation. Armfield have
developed an algorithm for the saponification reaction (ethyl acetate and sodium
hydroxide) linking the degree of conversion of the reactants to the electrical conductivity,
thus allowing the progress of the reaction to be monitored using the software.
The service unit includes a mounting position for the reactor being used. It is possible to
change reactors quickly and easily without the use of tools. All fittings on the CEXC and the
reactors are of the quick-release type. The CEM-MkII, CET-MkII and CEB-MkIII reactors are
completely contained on the CEXC base unit. The CEY and CEZ also include floor standing
columns for positioning next to the CEXC base unit.
The CEXC provides a locating position for two standard 2.5-litre chemical storage bottles
for the reagents within the plinth. This provides safety in use, and the bottles can be
quickly capped and removed as necessary for safe handling. Two 2.5-litre bottles are also
provided with the equipment. Alternatively, for longer experiments, larger feed vessels
could be located either on the floor or on the bench next to the equipment.
The CEXC requires a computer (not supplied by Armfield), running Windows XP or above,
with a spare USB port.

The CEB Transparent Batch Reactor is a double-skinned glass vessel with a one-litre
internal working volume, fitted with a variable-speed agitator.

CHEE3203P Reaction Engineering Practical Page 6

Hot water from the CEXC or cold water from the CW17 can be circulated through the
jacket for temperature control purposes, maintaining the reactor contents at constant
temperature.
Glands in the clear acrylic lid allow the CEXC conductivity and temperature probes to be
fitted to facilitate monitoring of the reactions in progress such as the important
saponification reaction. Isothermal and adiabatic operation reactions may be
demonstrated. (Note, the isothermal reaction requires the Armfield CW17 accessory if
experiments at low temperature are to be studied or if the ambient temperature is high).
For adiabatic operation, the use of dyes enables the chemical reaction rates to be
monitored visually by the change in colour at different degrees of conversion.
Key Features
 A small-scale batch reactor for use with the Chemical Reactors Service Unit designed
to demonstrate both adiabatic and isothermal operation (The Chilled Water
Circulation Unit accessory is recommended for isothermal operation)
 1l working volume
 The vessel includes a jacket through which hot water from the Chemical Reactors
Service Unit or chilled water from Chilled Water Circulation Unit is passed. A
variable-speed agitator aids heat transfer through the vessel
 The vessel is made of glass to give full visibility of the contents and allow the use of
colour tracers to illustrate the reaction process
 Fitting points for temperature and conductivity sensors (supplied with Chemical
Reactors Service Unit)
 Demonstration capabilities:
 Effect of temperature on reaction kinetics
 Effect of concentration on conversion
 Determination of the rate equation and activation energy through mass and energy
balances
 Study of temperature variation for exothermic reaction
 Use of colour tracers to illustrate reaction progress

CHEE3203P Reaction Engineering Practical Page 7

Theoretical Principles

As a rule, chemical processes are not spontaneous and are incomplete. Indeed, in the majority
of cases the reaction products only formed gradually. The speed of the reaction can be very
varied, as reactants only react with one another if they meet with a sufficiently large amount
of energy. An increase in the temperature, therefore increases the conversion of the
reactants. The time for which the reactants are in contact is a further criterion. The conversion
of the reactants is thus dependent on:
 The nature of the reactants
 The concentration and mixing of the reactant
 The time that the reactants are in contact
 The reaction temperature

These relationships are to be checked based on the saponification of Acetic Ether with
Sodium Hydroxide.
The following reaction occurs:

Acetic ether  Sodium hydroxide 

 ethanol  Sodium Acetate
CH 3 - COO - CH 2 CH 3  NaOH 
 CH 3 CH 2 - OH  CH 3 - COO - Na

The acetic ether molecules are split and each disintegrates into an acetate ion and an ethanol
molecule. During this process, the hydroxide ions in the sodium hydroxide are consumed. The
progress of the reaction and the conversion of the reactants can thus be tracked extremely
well by the change in the hydroxide concentration.

Alternatively, a conductivity measurement or volumetric analysis with acid can be used. From
the conductivity values, the percentage conversion of the reactants X can be calculated with
the aid of the following equation:
C  CA
X  A0 100%
CA0
CA: Actual measured value for conductivity at time t;
CA0: Initial conductivity of the sodium hydroxide at time = 0;

Or

(  e)
X 1 100%
o e
k: Actual measured value for conductivity;
ko: Initial conductivity of the 2.3% sodium hydroxide;
ke: Conductivity of the end product produced at time t.

CHEE3203P Reaction Engineering Practical Page 8

 Experiment 1

Chemical Reagent Preparation

Objective

Prepare the chemical solutions required for the reaction rate testing including a calibration
curve for the NaOH reagent.

What is MSDS?

Before start preparing the chemical reagents that will be used in the experiment, we need
to obtain the material safety data sheet (MSDS) for all reagents in the experiment.

A material safety data sheet is a technical document which provides detailed and
comprehensive information on a controlled product related to

 health effects of exposure to the product

 hazard evaluation related to the product’s handling, storage or use
 measure to protect workers at risk of exposure
 emergency procedures
The data sheet may be written, printed or otherwise expressed and must meet the
availability, design and content requirements of Workplace Hazardous Materials
Information System (WHMIS) legislation. The legislation provides for flexibility of design and
wording but requires that a minimum number of categories of information be completed
and that all hazardous ingredients meeting certain criteria be listed subject to exemptions
granted under the Hazardous Materials Information Review Act. The MSDS can be found
easily on the internet from different chemical supplier in different formats.
After reading the MSDS, we will be aware of the level of risk and required personal
protection when we handles these chemicals.

The reaction chosen for the isothermal demonstration is the saponification of ethyl acetate
by sodium hydroxide, as it can be carried out under safe conditions of temperature and
pressure and is well documented.

Dilution of Ethyl Acetate

use of a 0.1M solution of Ethyl Acetate, therefore add 4.895 ml of concentrated Ethyl
Acetate to 400 ml of deionised or distilled water. Shake the mixture vigorously until the two
liquids have mixed. Add further water to make up the final volume to 500 ml.

CHEE3203P Reaction Engineering Practical Page 9

Dilution of Sodium Hydroxide

use of a 0.1M solution of Sodium Hydroxide, this may be made by adding 50ml of NaOH 1M
to 450 ml of distilled water then making up the solution to 500ml.

https://web.microsoftstream.com/video/d836d4ca-d78a-4cc6-9ab1-28c443b30619

Preparation of NaOH calibration curve

https://web.microsoftstream.com/video/5fc04323-2965-4c1b-a09d-edf56531c293

Calibration curve is very useful tool in reading the change of the concentration of reactants
during the chemical reaction. In order to prepare the calibration curve, we need to prepare
different solutions of NaOH ranging from 0 – 0.1 M, such as (0 (pure water), 0.02, 0.04, 0.06,
0.08 and 0.1. Read the conductivity for each solution 3 times. Make a table as below.

NaOH (M) Conductivity 1 Conductivity 2 Conductivity 3 Average

Conductivity

0 0.9 0.89 1.00 0.93

0.02 7.06 7.20 7.15 7.14

0.04 9.00 9.05 9.04 9.03

0.06 13.25 13.3 13.35 13.30

0.08 19.99 20.0 19.99 20.00

0.10 23.75 23.99 23.99 23.91

Report 1:

After calculating the average conductivity, use excel sheet to plot Average conductivity vs
NaOH molarity. Later we will use this curve to convert the conductivity from experiment
into concentration.

What to include in my report?

1. Report is made by 3 members (maximum 6 pages A4 using MS Word). The
report should include cover page, summary, objectives, data collected, results and
discussions and conclusion. The report is written using 12pt Times New Romans.
Use 1.5 spacing, and 2.5 cm margins in all sides. The report is submitted in pdf
format. In the first page show the percent contribution for all members in the
team.
CHEE3203P Reaction Engineering Practical Page 10
 2. Write the experiment safety instructions and report from MSDS the safety for
handling the chemical reagents in the experimentations.
3. Show the data collected and the correlation between conductivity and molarity
(calibration curve)

CHEE3203P Reaction Engineering Practical Page 11

 Experiment 2

Finding the specific reaction rate

Objective

To find the reaction rate constant for the saponification of ethyl acetate with NaOH in a
constant volume batch reactor using integral method.

Procedure:
https://web.microsoftstream.com/video/1308222d-4d81-407e-bd55-f55f48ec2a88

1. Make up 0.5 liter of 0.1N sodium hydroxide and 0.5 liter of 0.1N ethyl acetate
2. Open Armfield Software and choose ‘Isothermal operation’. Set up the Hot Water
Circulator as detailed in the Operation section. Adjust settings on the PID loop as detailed
in Operation procedure for Isothermal Operation and set point to 25°C.
3. Charge the batch reactor with 0.5 liters of the sodium hydroxide solution. Set the reactor
agitator to '50%' and press ‘Power on’ to start the agitation. Then press ‘Hot Water
Circulator’ and water will start to recirculate through jacket reactor and vessel.
4. As the experiment involves the collection and storage of conductivity data, the data
output port in the plinth must be connected to the computer with Armfield Interface data
logger. This will enable data logging of the conductivity, temperatures and stirrer speed
values at selected time intervals over a selected period. Ensure the conductivity and
temperature sensors have both been installed in accordance with the Installation section.
Collection of data will be until a stable condition is reached in the reactor and this takes
approximately 30 minutes. It is advisable to set the data collection period to, say, 45
minutes.
5. Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in the
reactor vessel will begin to rise and will be automatically maintained at the desired set-
point (25oC in this instance) by the action of the HWC in the jacket. Carefully add to the
reactor 0.5 liters of the ethyl acetate solution and instigate the data logger program (or
begin taking readings if no computer is being used). It has been determined that the
degree of conversion of the reagents affects the conductivity of the reactor contents. By
recording the conductivity with respect to time, either manually or using the Armfield
Data Logger, the amount of conversion can be calculated.

https://web.microsoftstream.com/video/00ab3de6-6ed4-4d4b-b02b-cc1140e2d1e7

https://web.microsoftstream.com/video/91419c8d-c623-45bf-b5f6-666933f2e14c

https://web.microsoftstream.com/video/6e797f8e-7799-45f5-a714-f831807b4b4b

CHEE3203P Reaction Engineering Practical Page 12

Data sheet

Run No. 1
CA0 = 0.1
T=298K
Time (min) Conductivity
0 24
1 16
2 12.2
3 9.4
4 7.5
5 6.3
6 5.5

Report 2

1. Report is made by 3 members (maximum 6 pages A4 using MS Word). The

report should include cover page, summary, objectives, data collected, results and
discussions and conclusion. The report is written using 12pt Times New Romans.
Use 1.5 spacing, and 2.5 cm margins in all sides. The report is submitted in pdf
format. In the first page show the percent contribution for all members in the
team.
2. Show all data collected from experiment in tables
3. Show all calculations in MSword including all equations
4. Show how you get the answer for reaction constant k value and reaction order

CHEE3203P Reaction Engineering Practical Page 13

 Experiment 3
Finding the activation energy

Objective:
To study the effect of temperature on Arrhenius equation and evaluate the reaction
activation energy.

Repeat procedure of experiment 1 at another different temperature.

Procedure:
1. Make up 0.5 liter of 0.1N, solutions of sodium hydroxide and 0.5 liter of 0.1N ethyl
acetate
2. Open Armfield Software and choose ‘Isothermal operation’. Set up the Hot Water
Circulator as detailed in the Operation section. Adjust settings on the PID loop as
detailed in Operation procedure for Isothermal Operation and set point to 25°C.
3. Charge the batch reactor with 0.5 liters of the sodium hydroxide solution. Set the
reactor agitator to '50%' and press ‘Power on’ to start the agitation. Then press ‘Hot
Water Circulator’ and water will start to recirculate through jacket reactor and vessel.
4. As the experiment involves the collection and storage of conductivity data, the data
output port in the plinth must be connected to the computer with Armfield Interface
data logger. This will enable data logging of the conductivity, temperatures and stirrer
speed values at selected time intervals over a selected period. Ensure the conductivity
and temperature sensors have both been installed in accordance with the Installation
section. Collection of data will be until a stable condition is reached in the reactor and
this takes approximately 30 minutes. It is advisable to set the data collection period to,
say, 45 minutes.
5. Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in the
reactor vessel will begin to rise and will be automatically maintained at the desired
set-point (25oC in this instance) by the action of the HWC in the jacket. Carefully add
to the reactor 0.5 liters of the ethyl acetate solution and instigate the data logger
program (or begin taking readings if no computer is being used). It has been
determined that the degree of conversion of the reagents affects the conductivity of
the reactor contents. By recording the conductivity with respect to time, either
manually or using the Armfield Data Logger, the amount of conversion can be
calculated.
6. Repeat step 1 and 2 at temperature set point = 25C then continue to point 5.
7. Repeat step 1 and 2 at temperature set point = 50C then continue to point 5.

CHEE3203P Reaction Engineering Practical Page 14

Data sheet
Run No 1 Run 2
CA0 =0.1 CA0 =0.1
T1=298 T2=323
Time (s) Conductivity Time (s) Conductivity
0 24 0 24
1 16 1 15
2 12.2 2 11
3 9.4 3 8
4 7.5 4 7
5 6.3 5 5.8
6 5.5 6 5

Report 3

1. Report is made by 3 members (maximum 6 pages A4 using MS Word). The report

should include cover page, summary, objectives, data collected, results and discussions
and conclusion. The report is written using 12pt Times New Romans. Use 1.5 spacing,
and 2.5 cm margins in all sides. The report is submitted in pdf format. In the first page
show the percent contribution for all members in the team.
2. Show all data collected from experiment in tables
3. Show all calculations in MSword including all equations
4. Show how you get the answer for Arrhenius Constant and Activation Energy

CHEE3203P Reaction Engineering Practical Page 15

 Experiment 4
The initial rate method

Objective:

To study the effect of initial reaction concentration on calculating the reaction parameters
and finding the rate of reaction.

Procedure:
1. Make up 0.5 liter of 0.1N, solutions of sodium hydroxide and 0.5 liter of 0.1N ethyl
acetate
2. Open Armfield Software and choose ‘Isothermal operation’. Set up the Hot Water
Circulator as detailed in the Operation section. Adjust settings on the PID loop as
detailed in Operation procedure for Isothermal Operation and set point to 25°C.
3. Charge the batch reactor with 0.5 liters of the sodium hydroxide solution. Set the
reactor agitator to '50%' and press ‘Power on’ to start the agitation. Then press ‘Hot
Water Circulator’ and water will start to recirculate through jacket reactor and vessel.
4. As the experiment involves the collection and storage of conductivity data, the data
output port in the plinth must be connected to the computer with Armfield Interface
data logger. This will enable data logging of the conductivity, temperatures and stirrer
speed values at selected time intervals over a selected period. Ensure the conductivity
and temperature sensors have both been installed in accordance with the Installation
section. Collection of data will be until a stable condition is reached in the reactor and
this takes approximately 30 minutes. It is advisable to set the data collection period
to, say, 45 minutes.
5. Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in the
reactor vessel will begin to rise and will be automatically maintained at the desired
set-point (25oC in this instance) by the action of the HWC in the jacket. Carefully add
to the reactor 0.5 liters of the ethyl acetate solution and instigate the data logger
program (or begin taking readings if no computer is being used). It has been
determined that the degree of conversion of the reagents affects the conductivity of
the reactor contents. By recording the conductivity with respect to time, either
manually or using the Armfield Data Logger, the amount of conversion can be
calculated.
6. Repeat step 1 and 2 at temperature set point = 25C and NaOH concentration = 0.2
then continue to point 5.
7. Repeat step 1 and 2 at temperature set point = 25C and NaOH concentration = 0.3
then continue to point 5.

CHEE3203P Reaction Engineering Practical Page 16

Data sheet
Run No. 1 Run No. 3 Run No. 4
CA0,1 =0.1 CA0,2 =0.2 CA0,3 =0.3
T=298K T=298K T=298K
Time (s) Conductivity Time (s) Conductivity Time (s) Conductivity
0 24 0 38.4 0 48.9
1 16 1 23 1 28
2 12.2 2 19.5 2 24.3
3 9.4 3 15 3 19
4 7.5 4 12.3 4 15
5 6.3 5 9 5 11
6 5.5 6 8.2 6 10

Report 4

1. Report is made by 3 members (maximum 6 pages a4 using ms word). The report

should include cover page, summary, objectives, data collected, results and
discussions and conclusion. The report is written using 12pt times new romans. Use
1.5 spacing, and 2.5 cm margins in all sides. The report is submitted in pdf format.
In the first page show the percent contribution for all members in the team.
2. Show all data collected from experiment in tables
3. Show all calculations in MSword including all equations
4. Show how you get the answer for k-constant and reaction order.

CHEE3203P Reaction Engineering Practical Page 17