Reactor Lab Manual

Laboratory
Manual FACULTY OF ENGINEERING - SOHAR UNIVERSITY

CHEM4005
REACTION ENGINEERING(CHEM4005)
Course Coordinator: Dr. Ahmed Jawad Ali

Teaching Assistant :
Mrs. Saud
Mrs. Fatma Abdel Ameer
Reaction Engineering CHEM4005 1

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Table of Contents
Table of Contents Page

1. Introduction 3
2. General Instructions 3
3. Report Preparation Guidelines 4
4. Laboratory Safety Rules 7
5. Experiment 1 BATCH REACTOR 9
6. Experiment 2 CONTINUOUS STIRRED TANK REACTOR 15
7. Experiment 3 STIRRED TANK REACTORS IN SERIES 22
8. Experiment 4 TUBULAR REACTOR 27

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Introduction: This lab is one of the most important labs in the chemical engineering study. In
this lab, student will perform experiments to support their theoretical study of Batch, CSTR and
PFR reactors.
Objectives:
1- To familiarize students with main type of chemical reactors.

2- To analyze the experimental data to obtain the reaction rate expression (reaction order
and specific reaction rate constant).
3- Compare results obtained using different concentration measurement techniques.
4- Compare the conversion of reactants during a specification reaction in various types of
reactor.
5- Observe batch mixing under different operating conditions.
Contents:
4 existing Lab experiments, which are:
1. BATCH REACTOR
2. CONTINUOUS STIRRED TANK REACTOR
3. STIRRED TANK REACTORS IN SERIES
4. TUBULAR REACTOR
General Instructions
Comments
 ALL STUDENTS ARE REQUESTED TO ATTEND ALL EXPERIMENTS.
 One formal repot should be submitted by each group.
 Final exam will be written exam
Grading:
• Attendance & participation: 10 points
• Reports: 70 points
• Exam or presentation: 20 points
The above grading guideline is subject to change according to the instructor approach.

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Lab and Report Rules:
All students are expected to abide with the following requirements:
• Respecting all lab safety regulations
• Reading the experiment handout before performing the experiment, points will be
deducted for unprepared students
• Delayed reports will not be accepted, if accepted under special reasons, grade will be
diminished by 10% daily.
• Reports quality should meet the specification outlined in the report guidelines discussed
in the next section.
• Hand-written reports are accepted, however, typed is preferable.
• The layout and organization of the reports are very important, bad-looking and
unorganized reports may be subjected to grade deduction.
• The results whether in form of tables or figures should be very informative, clear and
precise that reflects the work of an Engineer.
• Figures should be very well labeled and scaled.
• The text should be written in the past tens or passive voice and avoid using the pronouns
I and/or We.
Report Preparation Guidelines

CHE4005 lab report must contain the following items in the order listed:
• Title
• Summary
• Objective
• Theory
• Procedure
• Results & discussion
• Conclusions
• Literature cited
• Nomenclature
• Appendices

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The following regulations should be taken care of while preparing a report, which define the
purpose of each item for the report contents:
Title page
The title page should be in a separate page and it must consists of the following:
• The name of the experiment
• The course number
• The name of students and their ID numbers
• The date when the experiment was run and the date of submission.
• The instructor name.
Summary
Summary section should be no more than one paragraph and it should summarize theMajor
results of the experiment. It can include the following items:
• Introduction to the subject of the specific experiment.
• Brief description of the work done.
• Numerical values of key results and findings.
Objective
Objective section should be 2-3 lines paragraph outlining the main objectives of the experiment.
The objective is not necessarily the same as the title.
Theoretical background
Theory section should be no less than a page and no more than 3 pages. In the section, the
necessary equations and derivations should be presented. Theory must be pertaining to the
experiment in hand.
Procedure
In this section, the student should list the actual step-by-step used to carry out the experiment.
The student should use his own wording or at least rephrase the procedure given in the handouts.

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Results and Discussion

The collected data and calculated results can be outlined in the form of neat Tables and Figures
for best demonstration. Discussion should contain your engineering analysis of unexpected,
abnormal or contradictory results and/or of experimental design or procedure deficiencies.
Interpretation of false results or mismatch between theoretical and experimental values can be
addressed in this section.
Conclusions
Conclusion should be no more than paragraph addressing the conclusive results of the
experiment. It should also highlight some of the interesting findings or problems encountered.
Similarly, special recommendations may be expressed if any. Conclusions and recommendation
should be written in an itemized format.
Literature cited
In this section, the student should list all books, Journal’s articles, etc. used in preparing the
report and analyzing the results. References must be arranged alphabetically by author’s name.
Nomenclature
An alphabetical list of all symbols, variables and abbreviations used in the report should be given
in this section. Proper units should be given whenever applicable.
Appendices
Appendix section can be added to include the raw experimental data, analyzed data, calculations,
etc. Any additional data or information should also be attached to the appendix.

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Laboratory Safety Rules
The laboratory rules apply to everyone using the lab, i.e., Professor, Instructors, Teaching
assistant, Technicians, and Students.
• Anyone running an experiment, in particularly students, must abide with the safety rules
posted around the labs.
• All personal belongings such as books, note books, etc... must be placed in the assigned
areas. These items must not be carried on during experiments.
• Smoking is strictly prohibited inside the laboratories. Similarly, eating or drinking is not
allowed.
• Laboratory Lab coat must be on at all times during experimentation sessions.
• Protective eye-glasses and gloves must be worn especially when handling chemicals.
• Students should not manipulate the laboratory equipment or their accessories unless
under the supervision of Lab personnel (Instructors, Technician).
• Students are requested to remain within their experiment vicinity and should not wander
around. Mingling with other groups is not recommended.
• Report any injuries regardless of its intensity.
• Report any equipment faults or safety hazards to lab personnel.
• Avoid unnecessary fluid leakage, waste of water, or waste of energy.
• Avoid inhalation of gases and vapors of any kind.
• In case of getting exposed to chemical spill, run to the emergency shower available in the
labs.
• At the end of the experiment, students are requested to clean the equipment and its
surrounding and return all apparatus to its normal places. Turn off the equipment and
disconnect the power supply.
• Remove all trash and place it in the receptacle.

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If any emergency arises call on the following numbers
EMERGENCY TELEPHONE NUMBERS:
Emergency Help:
Fire Department:
Campus Security:
STUDENT NAME : ____________________________
STUDENT ID NUMBER: _______________________
SEMESTER AND YEAR: ____________________

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Experiment #1
BATCH REACTOR
EXPERIMENTAL PROCEDURES
The Armfield batch reactor is designed to demonstrate the mechanism of a chemical reaction in a
reactor, as well as the effects of varying process conditions such as reaction temperature, reagent
concentrations etc.
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.
The reaction chosen for the adiabatic demonstration is the hydrolysis of acetic anhydride. This
involves the use of glacial acetic acid and sulphuric acid as well as acetic anhydride.
Although it may be possible to carry out demonstrations using other chemicals, it is not advisable
as the materials of construction of the reactor may not be compatible.
Before carrying out reactions involving any other reagents please refer to Armfield Ltd.
for advice.
DILUTION OF ETHYL ACETATE FOR USE WITH CEB MKII BATCH REACTOR
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CEB MkII
reactor. This should be made by diluting concentrated Ethyl Acetate as follows:
Therefore add 9.79 ml of concentrated Ethyl Acetate to 900 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 1000 ml.
Note: The practice of making a strong solution (e.g. 1M) then further diluting this to the required
concentration (e.g. 0.1M) cannot be applied when using Ethyl Acetate. The required dilution
should be made directly as stated above.

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DILUTION OF SODIUM HYDROXIDE FOR USE WITH CEB MKII BATCH REACTOR
Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CEB MkII reactor.
This may be made by adding 4.0g of NaOH to 960ml of deionised water then making up the
solution to 1000ml.
EXPERIMENT (A) ISOTHERMAL OPERATION
Note: This experiment requires the use of the Armfield Chilled Water Circulator accessory.
To find the reaction rate constant in a stirred batch reactor
The reaction:-
Assuming that the initial concentrations are equal and that the amount of reagent used up after
time t is X then the concentrations at time t are:
From the kinetic analysis of a general second order reaction it can be shown that:
where k is the reaction rate constant and t is the time of reaction. Using notation from the
nomenclature:
substituting for X in equation (1) above gives:
METHOD
Make up 0.5 litre batches of 0.1M sodium hydroxide and 0.1M ethyl acetate.
IMPORTANT: It is essential when handling these chemicals to wear protective clothing, gloves
and safety spectacles.
- Set up the Chilled Water Circulator as detailed in the CW-16 manual.
- Adjust the set point of the temperature controller to 15°C.

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- Switch the Heat/Chill switch on the CEX console to CHILL.
- Charge the batch reactor with 0.5 litres of the sodium hydroxide solution. Switch on
the reactor agitator and adjust the speed setting to '7.0'.
- As the experiment involves the collection and storage of conductivity data, the data
output port in the console must be connected to the Armfield IFD data logger and the
computer (as detailed in the instruction leaflet supplied with the interface). This will
enable data logging of the conductivity at selected time intervals over a selected
period. If a computer is not available then the conductivity can be recorded manually
at half minute intervals by reading the value directly from the conductivity meter in
the console.
- Ensure the conductivity probe and temperature sensor have both been installed in
accordance with the section CONNECTION TO SERVICES.
- 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.
- Switch on the chilled water circulator. The temperature of the sodium hydroxide in
the reactor vessel will begin to fall and will be automatically maintained at the desired
setpoint (150C in this instance) by the action of the chilled water circulating in the
submerged coil.
- Carefully add to the reactor 0.5 litres 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.
INTERPRETATION OF RESULTS
Having recorded the conductivity of the contents of the reactor over the period of the reaction,
the conductivity measurements must now be translated into degree of conversion of the
constituents.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution
whilst ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution at
a given concentration and temperature however, is not the same as that of a sodium acetate
solution at the same molarity and temperature and a relationship has been established allowing
conversion to be inferred from conductivity:-
The calculations are best carried out using a spreadsheet such as Microsoft™ Excel so that the
results can be displayed in tabular and graphical form.
On conclusion of the experiment, the set of readings of conductivity with time will need to be
transferred to the computer as two columns of data.
Now enter the following known constants from the experiment using the Nomenclature list on
last page. Ensure use of correct units.

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5. NOMENCLATURE

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Experiment #2
CONTINUOUS STIRRED TANK REACTOR
The Armfield continuous stirred tank reactor is designed to demonstrate the mechanism of a
chemical reaction in this type of reactor as well as the effects of varying the process conditions
such as reaction temperature, reactor volume, stirring rate, feed rate etc.
The reactor volume can be varied by adjusting the height of the internal standpipe. The actual
volume must be checked by filling the reactor with water to the overflow then draining the
reactor contents into a measuring cylinder.
Calibration of the feed pumps is achieved by pumping water from the reagent tanks to a
measuring cylinder over a timed period for a range of pump speeds. A calibration graph for each
pump of % speed vs. flowrate (ml/min) can then be drawn.
The conductivity of the reacting solution in the reactor changes with the degree of conversion
and this provides a convenient method for monitoring the progress of the reaction either
manually or by computer.
The reaction chosen 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.
The experiments involve the collection and storage of conductivity data. The data output port in
the console must be connected to the Armfield IFD data logger and the computer as detailed in
the instruction leaflet supplied with the interface. This will enable data logging of the
conductivity at selected time intervals over a selected period of time.
If a computer is not available then the conductivity can be recorded manually at half minute
intervals by reading the value directly from the conductivity meter in the console.
Although it may be possible to carry out demonstrations using other chemicals, it is not advisable
Before carrying out reactions involving any other reagents please refer to ArmfieldLtd.for
advice.

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DILUTION OF ETHYL ACETATE
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CEM MkII reactor.
This should be made by diluting concentrated Ethyl Acetate as follows:
DILUTION OF SODIUM HYDROXIDE

Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CEM MkII
reactor. This may be made by adding 4.0g of NaOH to 960ml of deionised water then making up
the solution to 1000ml.
OPERATION AS A BATCH REACTOR
If the unit is operated as a batch reactor (no continuous feed to the reactor) then temperature
control of the vessel contents will not be possible using the standard arrangement.
If it is required to operate in batch mode with the temperature elevated above ambient then the
temperature sensor should be removed from the gland in the top of the reactor and placed in the
vessel on the side of the hot water circulator. The temperature controller will then regulate the
temperature of the water flowing through the heating coil, preventing overshoot and maintaining
the vessel contents at a steady value. The actual temperature of the vessel contents can be
monitored using a spirit filled glass thermometer (not supplied) through the vacant gland in the
lid. Any small offset in the actual temperature of the reactor contents can be compensated by
changing the set point on the controller by a corresponding amount.
As the standard reaction is exothermic the heat generated by the reaction will result in a rise in
temperature of the vessel contents that is unavoidable. If it is required to maintain the reaction at
a more precise temperature then it will be necessary to perform the trial at a temperature below
the ambient temperature using the optional chilled water circulator CW-16 (not supplied)
connected to the coil in the reactor vessel.
EXPERIMENT A
To find the reaction rate constant in a Continuous Stirred Tank Reactor THEORY
The reaction:-

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can be considered equi-molar and first order with respect to both sodium hydroxide and ethyl
acetate, i.e. second order overall, within the limits of concentration (0 - 0.1M) and temperature
(20 - 40°C) studied.
The reaction carried out in a Continuous Stirred Tank Reactor or Tubular Reactor eventually
reaches steady state when a certain amount of conversion of the starting reagents has taken place.
The steady state conditions will vary depending on concentration of reagents, flowrate, volume
of reactor and temperature of reaction.
METHOD
Remove the lids of the reagent vessels and carefully fill with the reagents to a level
approximately 50mm from the top. Refit the lids.
Adjust the set point of the temperature controller to 30°C.
Collection of conductivity data will be until a steady state 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.
Using the calibration graph for each of the feed pumps, set the pump speed control to give 40
ml/min flowrate.
Set the agitator speed controller to 7.0.
Switch on both feed pumps and the agitator motor, and instigate the data logger program (or
begin taking readings if no computer is being used). After a few minutes the temperature sensor
tip will be covered (about 25mm of liquid in reactor) – switch on the hot water circulator.
It has been determined that the degree of conversion of the reagents affects the conductivity of
the reactor contents so that recording the conductivity with respect to time using the Armfield
data logger can be used to calculate the amount of conversion.
INTERPRETATION OF RESULTS.
Having recorded the conductivity of the contents of the reactor over the period of the reaction,
the conductivity measurements must now be translated into degree of conversion of the
constituents.
a given concentration and temperature, however, is not the same as that of a sodium acetate
conversion to be inferred from conductivity.
The calculations are best carried out using a spreadsheet such as EXCEL so that the results can
be displayed in tabular and graphical form.

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On conclusion of the experiment using the Armfield data logger, a set of readings of conductivity
with time will be stored in the computer.
At this point, this data can be transferred onto the spreadsheet.
Start the spreadsheet program.
last page. Ensure use of correct units.

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5.7 Nomenclature

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Experiment 3:
STIRRED TANK REACTORS IN SERIES
EXPERIMENT E
Demonstration of the progress of a second order chemical reaction through three
continuous stirred tank reactors connected in series
THEORY
The reaction:-
acetate i.e. second order overall, within the limits of concentration (0 - 0.1M) and temperature
The reaction carried out in a Continuous Stirred Tank Reactor eventually reaches steady state
when a certain amount of conversion of the starting reagents has taken place.
METHOD
Collection of conductivity data will be until a steady state condition is reached in the reactor and
this takes approximately 45 minutes. It is advisable to set the data collection period to, say, 60
minutes.
Using the calibration graph for each of the feed pumps, set the pump speed controls to give 60
ml/min flowrate.
Set the agitator speed controller to 7.0.

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Switch on both feed pumps and agitator motor, and instigate the data logger program (or begin
taking readings if no computer is being used).
data logger can be used to calculate the amount of conversion.
Having used the Armfield data logger CEX-304IFD to record the conductivity of the contents of
the reactors over the period of the reaction, the conductivity measurements are automatically
translated into degree of conversion of the constituents.
conversion to be inferred from conductivity.
Comment upon the results obtained.
If readings have been obtained manually then the necessary calculations are best carried out
using a spreadsheet such as EXCEL so that the results can be displayed in tabular and graphical
form. On conclusion of the experiment the recorded data can be transferred into the spreadsheet.
Enter the following known constants from the experiment using the Nomenclature list on page
E-6. Ensure use of correct units.

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For the values of each of the above, the spreadsheet can be used to calculate values of sodium
hydroxide concentration (a1) and sodium acetate concentration (c1) and the degree of conversion
(Xa) and (Xc) for each of the samples of conductivity taken over the period of the experiment.
These can be calculated and listed in columns (use spreadsheet COPY facility) alongside the
readings of conductivity using the following equations:-

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NOMENCLATURE

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Experiment 4
TUBULAR REACTOR
The Armfield Continuous Tubular Flow Reactor is designed to demonstrate the mechanism of a
chemical reaction in such a reactor as well as the effects of varying the process conditions such
as reaction temperature, reactant concentration, feed rate etc.
The reaction chosen 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.
Although it may be possible to carry out demonstrations using other chemicals it is not advisable
Before carrying out reactions involving any other reagents please refer to ArmfieldLtd.for
advice.
DILUTION OF ETHYL ACETATE FOR USE WITH CET MKII REACTOR
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CET MkII reactor. This
should be made by diluting concentrated Ethyl Acetate as follows:
DILUTION OF SODIUM HYDROXIDE FOR USE WITH CET MKII REACTOR

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Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CET MkII reactor.
This may be made by adding 4.0g of NaOH to 960ml of deionised water then making up the
solution to 1000ml.
EXPERIMENT A
To determine the rate constant using a tubular reactor
THEORY
acetate i.e. second order overall, within the limits of concentration (0 - 0.1M) and temperature
The reaction carried out in a Continuous Stirred Tank Reactor or Tubular Reactor eventually
reaches steady state when a certain amount of conversion of the starting reagents has taken place.
METHOD

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Adjust the set point of the temperature controller to 25°C.
As the experiment involves the collection and storage of conductivity data, the data output port
in the console must be connected to the Armfield IFD data logger and the computer as detailed in
the instruction leaflet supplied with the interface. This will enable data logging of the
conductivity at selected time intervals over a selected period.
If a computer is not available then the conductivity can be recorded manually at half minute
intervals, by reading the value directly from the conductivity meter in the console.
Ensure the conductivity probe and temperature sensor have been installed in accordance with the
section CONNECTION TO SERVICES.
Collection of data will be until a steady state 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.
Using the calibration graph for each of the feed pumps, set the pump speed controls to give 80
ml/min flowrate for each reactant (Fa = Fb = 80ml/min = 1.33 x 10-3 dm3/sec.)
Prior to priming the hot water circulating pump, fill the reactor with cold water. To fill the
vessel, it is necessary to pinch together the walls of the tubing connecting the overflow to the hot
water circulator, either manually by bending and holding the tube or using a suitable clip
(ensuring that any clip used will not cause damage to the tubing).
Fill the vessel to a level above the overflow (return to the circulator), just below the reactor lid,
using a suitable hose from a domestic supply through the temperature sensor gland (8) in the lid.
A non-return valve (11) prevents water flowing out of the reactor via the inlet. Ensure the
temperature sensor is re-fitted and the gland tightened securely by hand before releasing the
outlet tubing.
Prime the pump as detailed in the OPERATIONAL PROCEDURES section of the CEX manual.
Switch on the hot water circulator. The temperature of the water in the reactor vessel will begin
to rise and will be automatically maintained at the desired set-point (250C in this instance).
Switch on both feed pumps and instigate the data logger program (or begin taking readings if no
computer is being used).
Reactants will flow from both feed vessels and enter the reactor through the connections in the
lid. Each reactant passes through pre-heat coils submerged in the water in which they are
individually brought up to the reaction temperature. At the base of the tubular reactor coil, the
reactants are mixed together in a "T" connection and begin to pass through the coil. The reacting
solution will emerge from the coil through connector (16) in the lid where a probe senses
continuously the conductivity which is related to degree of conversion.
Data Logger can be used to calculate the amount of conversion.

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The conductivity measurements must now be translated into degree of conversion of the
constituents.
conversion to be inferred from conductivity:-
The calculations are best carried out using a spreadsheet such as EXCEL so that the results can
be displayed in tabular and graphical form.
On conclusion of the experiment using the Armfield data logger, a set of readings of conductivity
with time will be stored in the computer.
At this point, this data can be transferred onto the spreadsheet.
Start the spreadsheet program.
page C2. Ensure use of correct units.

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Comment upon the results obtained.

Notes:
1. It is recommended that this experiment should be repeated at various other temperatures
to investigate the relationship between the specific rate constant (k) and the temperature
of reaction.
2. It is further recommended that the experiment be repeated using dissimilar flow rates for
the caustic soda and ethyl acetate solutions to investigate the effect that this will have
upon the saponification process.
Rinse the feed tanks with demineralised water and pump the water through the reactor to
rinse out the chemicals. The reactor can be left with water in the coil ready for the next
experiment.
When removing the CET reactor from the service unit always drain using the drain valve
under the baseplate first.

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6. NOMENCLATURE

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Laboratory

Manual FACULTY OF ENGINEERING - SOHAR UNIVERSITY

Course Coordinator: Dr. Ahmed Jawad Ali

Reaction Engineering CHEM4005 1

Table of Contents Page

Reaction Engineering CHEM4005 2

1- To familiarize students with main type of chemical reactors.

Reaction Engineering CHEM4005 3

Report Preparation Guidelines

Reaction Engineering CHEM4005 4

Reaction Engineering CHEM4005 5

Results and Discussion

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Reaction Engineering CHEM4005 7

EMERGENCY TELEPHONE NUMBERS:

STUDENT NAME : ____________________________

STUDENT ID NUMBER: _______________________

SEMESTER AND YEAR: ____________________

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EXPERIMENT (A) ISOTHERMAL OPERATION

substituting for X in equation (1) above gives:

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DILUTION OF SODIUM HYDROXIDE

OPERATION AS A BATCH REACTOR

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DILUTION OF ETHYL ACETATE FOR USE WITH CET MKII REACTOR

DILUTION OF SODIUM HYDROXIDE FOR USE WITH CET MKII REACTOR

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To determine the rate constant using a tubular reactor

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Comment upon the results obtained.

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