Laboratory Manual Feb 2023
Laboratory Manual Feb 2023
Each experimental report should include the following items in the order listed:
1. Cover Page (All)
Please insert the LABORATORY REPORT SUBMISSION FORM as the front cover.
2. Table of Contents (All)
The table of contents and page number should be as follows.
Content Page Number
Summary
1.0 Results and Discussion
2.0 Conclusions and Recommendations
3.0 Tutorial
4.0 References
5.0 Appendices
3. Summary (Student 1)
Provide a summary of the overall experimental report (half a page). Review the experiment’s objectives
main results and discussions, and finally the conclusions.
4. Results (Student 1)
Refer the respective experimental procedure (Analysis and Discussion sections) for details.
a. Properly record and present all experimental data, findings, and calculations.
b. Present the data either in Table, Graph, Histogram, or Pie chart form with complete labelling and
units.
Example Table:
Table 1: X vs. Y
Samples X (unit) Y (unit)
A
B
C
D
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Example Figure:
5. Discussions (Student 2)
a. Table and figure explanation
b. Discuss on your findings in relation to the theory and the experiment’s objectives
6. Conclusions and Recommendations (Student 3)
a. Summary of the results to briefly relate the findings or results to the experimental theory and
objectives
b. Suggest improvements in equipment or measurement procedures, or even experimental procedures
for future work (if applicable).
c. In one paragraph.
7. Tutorial (Student 4)
Tutorials are questions in laboratory manual. All questions must be answered.
8. References (All)
Source of material cited in the text. The references should be arranged alphabetically by author. Format
the references as follows:
1. Books/Journals: Authors (editor), title, publisher, year, chapter or page number
Example: Smith J.M. and Van Hess H.C., Introduction to Chemical Engineering Thermodynamics,
McGraw-Hill, New York, 2001, p229
2. Internet Website: Title of the information, year, source of data, [Online]. [Date Accessed].
Available from World Wide Web
Example: BP Statistical Review of World Energy, 2007, BP (British Petroleum), [Online].
[Accessed 19th January 2008]. Available from World Wide Web: http://bp.com/statisticalreview.
9. Appendices (All)
This should contain all raw data and a calculation sample. Students may handwrite the calculations. The
rest of the report should be typed.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
APPENDIX
CHEMICAL PREPARATION
V 1 ( L )=
M2( molL )V ( L )
2
10.10 (
L )
mol
Where;
M2 = Desired molarity of Ethyl Acetate (mol/L) required in the experiment
V2 = Desired volume of Ethyl Acetate (mol/L) required in the experiment
Where;
M2 = Desired molarity of NaOH (mol/L) required in the experiment
V2 = Desired volume of NaOH (mol/L) required in the experiment
Molecular weight of NaOH, MWNaOH = 40.0 g/mol
V 1 ( L )=
M2( molL )V ( L )
2
1.0 (
L )
mol
Where;
M2 = Desired molarity of HCl (mol/L) required in the experiment
V2 = Desired volume of HCl (mol/L) required in the experiment
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
LABORATORY MANUAL
REACTION ENGINEERING (CKB 20104)
LIST OF EXPERIMENTS:
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
GENERAL DESCRIPTION
Description and Assembly
Before operating the unit and running experiments, you must familiarize yourself with the unit’s
components. Please refer to Figure 2 to understand the process. All glass components of the QVF Batch
Reactor unit are made of borosilicate glass with PTFE gaskets.
1. Reactor (R1)
Fused jacketed vessel with graduation, nominal capacity 10 L
Bottom port for dead space reduced bottom outlet valve
Jacket connections for heating agent
Cover DN300 with connections for: Agitator
Charge port with screw cap for feeding by hand
Inlet for dosing vessel B1
Vapour pipe with connection for distillate and vapour trap
Conductivity and temperature sensor
2. Agitator (A1)
Laboratory drive 230V / 50,60Hz
0.25 kW, 0-550 rpm, steplessly adjustable by hand
3. Dosing vessel (B1)
2,000 mL graduated cylindrical vessel with overflow pipe
4. Condenser (W1)
Coil heat exchanger, area 0.3 m2
Max coolant pressure of 3 bars with allowable temperature difference of 130°C
5. Instrumentation
Temperature measurement (TI-101)
Conductivity measurement (QI-401)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Chemical engineering processes can be broadly divided into two types: batch processes and continuous
processes. In a batch process, input materials are placed in a reactor and product is withdrawn sometime
later. This is typical of what is normally done in chemistry laboratories. You will be studying for batch
conditions the reaction between an ester (ethyl acetate) and sodium hydroxide:
CH3COOC2H5 + OH- CH3COO- + C2H5OH
This type of reaction is called a saponification because of its importance in the manufacture of soap. The
reaction is relatively slow, and the changing ester concentration can be followed quite easily by analysing
samples from the reaction mixture every few minutes. The second order rate constant is determined in two
different ways:
dt
Separating the variables and integrating with appropriate boundary conditions,
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
CA t
dCA
∫ CA
2
=k ∫ dt
C A0 0
1 1
=kt+
CA C A0
A plot of 1/CA against t (reaction time) should give a straight line with the gradient, k (reaction rate
constant).
2. Half-life method
From
1
CA
=kt+
1
C A0
can be rearranged to give k = (
1 C A 0−C A
t CA C A0 )
C A0
Let t1/2 be the time taken for the concentration of ester to be halved, C A=
2
1
Then k = t C
1 /2 A 0
The time taken to halve the concentration of ester is inversely proportional to the initial concentration, C A0.
From plot of the ester concentration C A against t (reaction time), it is possible to determine t 1/2 and hence the
k (reaction rate constant).
Safety Consideration
1. Students must not carry out laboratory work without the supervision of a lecturer.
2. Read the operating instructions carefully, and make sure you understand all aspects of the operation of
the batch reactor unit.
3. All experiments must be conducted with safety glasses on at all times.
4. Allow 10 minutes for each experimental conditions to reach equilibrium.
5. After each experiment, make sure that the reactor and tubing are cleaned properly. Sodium hydroxide
and ethyl acetate both are corrosive and can damage the tubing’s and the reaction rig.
6. Dispose all liquids immediately after each experiment. Do not leave any reactants or product in the feed
or product vessels.
7. Wipe off any spillage on the ground or working bench.
8. Plastic gloves and eye shields must be worn when handling corrosive liquids and heat resistant gloves
when adjusting steam valves.
9. All experiments involving a potential explosive hazard must be conducted behind special shields.
10. When working with solvents etc., ensure that the apparatus is adequately vented.
11. All used solvent should be handed to the technician and not disposed into drains or laboratory sinks.
12. Smoking is forbidden in all laboratories.
13. Safety helmets must be worn.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
14. Services equipment (vacuum generators) must in no circumstances be started up by students.
15. Gas cylinders, when in use, should be adequately strapped to bench and supported in the upright
position, away from sunlight or flames. Ensure that cylinders are shut-off after use.
16. Before using any chemical, ensure that you are familiar with its hazards and with emergency
procedures.
17. If in doubt, ask the lecturer in charge.
18. If chemical spillage occurs, evacuate the laboratory in an orderly fashion.
19. Plug in all cables into appropriate sockets before switching on the main switch. Inspect all cables for
any damage to avoid electric shock. Replace if necessary.
20. Do not switch on the heater unless it is fully submerged in the liquid. Always maintain liquid level
above the height of the heater to avoid damage to the heater.
EXPERIMENTAL PROCEDURES
1. Prepare the following solutions:
a) 9 L of sodium hydroxide, NaOH (0.1 M)
b) 9 L of ethyl acetate, Et (Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Turn on the power for the control panel.
4. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
5. Open cooling water valve V5 and let the cooling water flow through the condenser W1.
6. Switch on the thermostat T1 and set the water temperature to the desired temperature (40C).
7. The unit is now ready for experiment.
8. Measure and carefully pour 3 L of 0.1 M ethyl acetate solution into the reactor R1 through the charge
port on the vessel cover.
9. Then, measure and carefully pour 3 L of 0.1 M sodium hydroxide solution into the reactor R1 through
the charge port on the vessel cover.
10. Switch on the stirrer M1.
11. Start the timer simultaneously.
12. At every 5-minute interval, open sampling valve V1 (at the bottom) and collect a 10 mL sample. Carry
out a conductivity measuring by using conductivity meter.
13. Record your conductivity and temperature from TI-101 in the Appendix C.
14. End the experiment when the conductivity values do not change significantly over time. Switch off the
stirrer M1. Drain the reactor R1 by opening valve V1.
15. Refilled the reactor with fresh solutions of 3 L of 0.1 M ethyl acetate and 3 L of 0.1 M sodium
hydroxide.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
16. Repeat the experiment (steps 1-8) for different reactor temperature by setting the thermostat temperature
to the assigned temperature (check schedule).
17. Perform the general shutdown procedures.
RESULTS
1. Use the sample table in Appendix B for data collection.
2. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis) using
Appendix A.
3. Calculate the concentration of NaOH, CNaOH from the calibration curve. Calculate the conversion, X based
on the formula given in Appendix B.
4. Plot conversion, X vs reaction time, t for the different temperatures.
5. Plot 1/CNaOH versus reaction time, t to get a straight line with a gradient equal to k at each temperature.
Determine the gradient to obtain the rate constant, k for each temperature. The rate law for a second
order reaction is given as
1 1
=kt+
C NaOH C NaOH , 0
−Ea
6. Plot ln k vs 1/T to get a straight line with the gradient equal to and y-intercept equal to ln A.
R
In linear form, ln k =
R T( )
−Ea 1
+lnA (R = 8.314 J/mol.K)
7. Calculate saponification activation energy, Ea and frequency factor, A from slope and y-intercept.
DISCUSSION
1. Discuss the experimental work.
2. Discuss the plot conversion, X versus reaction time, t and compare the conversions for the different
temperature. Discuss it thoroughly including how temperature affects the reaction.
3. Examine the reaction rate constant change with temperature.
4. Discuss the saponification activation energy, Ea and frequency factor, A
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
TUTORIAL
1. Describe an industrial process other than saponification that uses batch reactor. Discuss thoroughly the
benefits and drawbacks of batch reactor in the process.
2. Write a one-paragraph summary of any journal article on batch reactor reaction. The article must be
published within 2020-2022. Explain the batch reactor used in the study and its significance.
APPENDIX A TABLE OF CALIBRATION CURVE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Use the calibration curve to determine the concentration of NaOH in the experiment.
REFERENCES
7.0 Atkins, P.W. ‘Physical Chemistry’ (various ed.)
8.0 Smith, J.M. ‘Chemical Engineering Kinetics ‘(3rd ed.), McGraw-Hill, 1981
9.0 Frost, A.A. & Pearson, R.G. ‘Kinetics and Mechanics’ (2nd ed.), Wiley, 1961
10.0 Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd edition, Prentice Hall Int. Series, N.J.
(USA), 1997.
11.0 Levenspiel, O., Chemical Reaction Engineering, 3rd edition, John Wiley and Sons, 1999
12.0 Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
GENERAL DESCRIPTION
Description & Assembly
Before operating the unit and running experiments, you must familiarize yourself with the unit’s
components. Please refer to Figure 1 to understand the process. All glass components of the QVF
Continuous Stirred Tank Reactor unit are made of borosilicate 3.3 glass with PTFE gaskets.
1. Reactor (R1)
Fused jacketed vessel with graduation, nominal capacity 10 L
Bottom port for dead space reduced bottom outlet valve
Jacket connections for heating agent
Cover DN300 with connections for Agitator, Charge port with screw cap for feeding by hand, Inlet
for feed vessels B1 and B2, Vapour pipe, and Integrated conductivity and temperature sensor
2. Agitator (A1)
Laboratory drive 230V / 50,60Hz
0.11 kW, 50-700 rpm, steplessly adjustable by hand, max torque 60 Ncm
3. Feed vessels (B1/B2)
50 L graduated cylindrical vessels
4. Pumps (P1/P2)
Centrifugal pumps
Max suction height of 3 m
5. Condenser (W1)
Coil heat exchanger, area 0.2 m2
Max coolant pressure of 2 bar with allowable temperature difference of 150°C
6. Receiving vessel (B3)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
100 L rectangular tank
7. Instrumentation
Flow measurement (FI-301, FI-302)
Temperature measurement (TI-101)
Conductivity measurement (QI-401)
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff who has been properly trained to
handle the unit.
2. All operating instructions supplied with the unit must be carefully read and understood before
attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be used.
4. The system should not be subjected to shock, sudden impact, vibration, additional load, or permanent
external action of aggressive vapours.
5. Always check and rectify any leakages.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top condenser (W3) and product
cooler (W4).
11. Only a properly trained staff should be allowed to carry out any servicing. Manufacturer's manual must
always be observed.
12. Before any servicing, shut down the whole operation, let the system cool down and be properly
ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or seals if necessary.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
EXPERIMENTAL PROCEDURES
1. Prepare the following solutions:
a) 30 L of sodium hydroxide, NaOH (0.1 M)
b) 30 L of ethyl acetate, Et(Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Charge the feed vessels as follows:
a) Open the charge port caps for vessels B1 and B2.
b) Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution into vessel B2.
c) Close the charge port caps for both vessels.
4. Turn on the power for the control panel.
5. Open valves V2, V7, and V11.
6. The unit is now ready to be used for an experiment.
7. Switch ON both pumps P1 and P2 simultaneously.
8. Open and adjust the valves V5 (Monitor at FI-301) and V10 (Monitor at FI-302) to give a flow
rate of about 150 mL/min. Both must be adjusted to equal flow rate.
9. Let the reactor fill up with both solutions until it is just about to 1/2 full.
10. Switch ON the stirrer M1.
11. Adjust the valves V5 and V10 to give the desired flow rate. Make sure that both flow rates are
maintained the same.
12. Start monitoring the conductivity value at QI-401.
13. Start the timer and record the conductivity value (QI-401) and both flow rates (FI-301 and FI-302)
when it has reached steady state (Conductivity value begin to steadily decline with time).
14. Record the conductivity values and both flows rate for every 5 minutes until the conductivity does
not change over time. This is to ensure that the reactor has reached steady state.
15. End the experiment when the conductivity values do not change significantly over time.
16. Repeat the experiment (steps 8 to 15) for different residence times by adjusting the feed flow rates
of NaOH and Et(Ac) to the assigned flow rate (Check schedule)
17. Make sure that both flow rates are maintained the same.
DISCUSSION
1. Discuss experimental work.
2. Discuss the plot conversion, X versus reaction time, t and compare the conversions for the
different resident times. Discuss it thoroughly, including how residence time affects the reaction.
3. Discuss how residence time can influence the rate constant, k, and the rate of reaction, –rNaOH.
TUTORIAL
1. Describe an industrial process other than saponification that uses CSTR. Discuss thoroughly the
benefits and drawbacks of the reactor in the process.
2. Write a one-paragraph summary of any journal article on CSTR reaction. The article must be
published within 202-2021. Explain the CSTR used in the study and its significance.
REFERENCES
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA), 1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall (USA), 1999.
3. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore), 1981.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Use the calibration curve to determine the concentration of NaOH in the experiment.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
GENERAL DESCRIPTION
Description and Assembly
Before operating the unit and running experiments, students must familiarize themselves with the
unit’s components. Please refer to Figure 1 to understand the process. All glass components of the
QVF Plug Flow Reactor unit are made of borosilicate 3.3 glass with PTFE gaskets.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff that has been properly
trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and understood before
attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be used.
4. The system should not be subjected to shock, sudden impact, vibration, additional load, or
permanent external action of aggressive vapors.
5. Always check and rectify any leak.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top condenser (W3) and product
cooler (W4).
11. Only a properly trained staff shall be allowed to carry out any servicing. Manufacturer's manual
must always be observed.
12. Before any servicing, shut down the whole operation and let the system to cool down and be
properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or seals if necessary.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
EXPERIMENTAL PROCEDURES
1. Prepare the following solutions:
a) 50 L of sodium hydroxide, NaOH (0.1 M)
b) 50 L of ethyl acetate, Et(Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Fill the feed vessel B1 with the NaOH and feed vessel B2 with the Et(Ac) solution.
4. Turn on the power for the control panel.
5. Open valves V1 and V2.
6. Switch on pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions into the dosing
vessels HB1 and HB2 towards valves V8 and V7.
7. Make sure that the pipelines before valves V7 and V8 are filled with solutions. Bleed any trapped
air in the pipelines by using valves V7 and V8.
8. Allow both the solutions to overflow in the dosing vessels HB1 and HB2 into the feed vessels B1
and B2.
9. The unit is now ready for experiment.
10. Open valves V7 and V8 and adjust valves V7 (Monitor at FI-301) and V8 (Monitor at FI-302) to
give a flow rate of about 200 mL/min. Make sure that both flow rates are the same.
11. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and empty into the
receiving vessel B3.
12. Adjust valves V7 and V8 to give the desired flow rate. Make sure that both flow rates are the
same.
13. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
14. Start the timer and record both conductivity values (QI-401 and QI-402) and flow rates (FI-301
and FI-302) when it has reached steady state (Conductivity value begin to steadily decline with
time).
15. Record the inlet and outlet conductivity values and both flow rates for every 5 minutes until the
conductivity do not change over time. This is to ensure that the reactor has reached steady state.
16. Repeat the experiment (steps 4 to 5) for different residence times by adjusting the flow rates to the
assigned flow rate (check schedule). Make sure that both flow rates are the same.
RESULTS
1. Use the table for data collection at Appendix B.
2. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis) using
Appendix A.
3. Calculate the concentration of NaOH, CNaOH from the calibration curve. Calculate the conversion, X
based on the formula given in Appendix.
4. Plot conversion, X vs reaction time, t for the different residence time.
5. The reactor’s residence time is defined as the reactor volume divided by the total feed flow rates,
F0. Calculate the average residence time, τavg for each flow rate.
V CSTR
Residence Time , τ=
F0
6. Calculate the reaction rate constant, k, and the rate of reaction, –r NaOH using the average residence
time, τavg for each flow rate.
C NaOH ,0 −C NaOH
Reactionrate constant , k= 2
τ avg C NaOH
DISCUSSION
1. Discuss experimental work.
2. Discuss the plot conversion, X versus reaction time, t and compare the conversions for the
different resident times. Discuss it thoroughly, including how residence time affects the reaction.
3. Discuss how residence time can influence the rate constant, k, and the rate of reaction, –rA.
TUTORIAL
1. Describe an industrial process other than saponification that uses PFR. Discuss thoroughly the
benefits and drawbacks of the reactor in the process.
2. Write a one-paragraph summary of any journal article on PFR reaction. The article must be
published within 202-2021. Explain the PFR used in the study and its significance.
REFERENCES
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA), 1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall (USA), 1999.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Use the calibration curve to determine the concentration of NaOH in the experiment.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Total flow
Inlet Outlet
rate of Residence
Flow rate Flow rate concentration concentration Conversion,
solutions, time, τ Inlet Outlet
Temperature of NaOH, of Et(Ac), of NaOH, of NaOH, X (%)
Time F0 (mL/min) (min) conductivity Conductivity
(°C) FNAOH FET CNaOH (M) CNaOH (M) (Self-
(min) = FNAOH + FET (Self- (mS/cm) (mS/cm)
(mL/min) (mL/min) (Calibration (Calibration calculate)
(Self- calculate)
curve) curve)
calculate)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
F0,avg = τavg =
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Total flow
Inlet Outlet
rate of Residence
Flow rate Flow rate concentration concentration Conversion,
solutions, time, τ Inlet Outlet
Temperature of NaOH, of Et(Ac), of NaOH, of NaOH, X (%)
Time F0 (mL/min) (min) conductivity Conductivity
(°C) FNAOH FET CNaOH (M) CNaOH (M) (Self-
(min) = FNAOH + FET (Self- (mS/cm) (mS/cm)
(mL/min) (mL/min) (Calibration (Calibration calculate)
(Self- calculate)
curve) curve)
calculate)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
F0,avg = τavg =
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
GENERAL DESCRIPTION
Description and Assembly
Before operating the unit and running experiments, you must familiarize yourself with the unit’s
components. Please refer to Figure 1 to understand the process. All glass components of the QVF
Reactor Test Rig unit are made of borosilicate 3.3 glass with PTFE gaskets.
1. Reactor (R1)
Jacketed cylindrical vessel, 4 L nominal capacity
2. Cascaded reactors (R2/R3/R4)
Jacketed cylindrical vessel, 1 L nominal capacity each
3. Plug flow reactor (SR1)
Jacketed pipe with approximate capacity of 3.0 L
4. Feed vessels (B1/B2)
100 L PE rectangular vessels with all necessary connections
5. Dosing vessels (HB1/HB2)
1 L cylindrical vessels with overflow port and bottom port
6. Pumps (P1/P2)
Centrifugal pumps
max delivery rate of 60 L/h and max delivery height of 8 m
7. Pre-heater (W1/W2)
Coil heat exchanger, area 0.06 m2
max heating media pressure of 0.5 bar
8. Receiving vessel (B3)
100 L rectangular tank
9. Instrumentations
Flow measurements (FI-301, FI-302, FI-303)
Temperature measurements (TI-101, TI-102, TI-103, TI-104)
Conductivity measurements (QI-401, QI-402, QI-403, QI-404)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff that has been properly
trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and understood before
attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be used.
4. The system should not be subjected to shock, sudden impact, vibration, additional load, or
permanent external action of aggressive vapours.
5. Always check and rectify any leak.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top condenser (W3) and product
cooler (W4).
11. Only a properly trained staff shall be allowed to carry out any servicing. Manufacturer's manual
must always be observed.
12. Before any servicing, shut down the whole operation and let the system to cool down and be
properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or seals if necessary.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
11. Start the timer and record both conductivity values (QI-401 and QI-403) and flow rates (FI-302
and FI-303) when it has reached steady state (Conductivity value begin to steadily decline with
time).
12. Record the inlet and outlet conductivity and flow rate of the reactor for every 5 minutes until they
do not change over time. This is to ensure that the reactor has reached steady state.
Shut-Down Procedure
1. Switch off both pumps P1 and P2.
2. Close the process water valve V27.
3. Open valves V3 to V21 and valve V26 to drain all liquid from the unit.
4. Turn off the power for the control panel.
RESULTS
1. Use the sample table in Appendix B for data collection.
2. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis) using
Appendix A.
3. Calculate the concentration of NaOH, CNaOH from the calibration curve. Calculate the conversion,
X based on the formula given in Appendix.
4. Plot conversion, X vs reaction time, t for each of the reactor.
5. Calculate the following parameter for the Single Stage CSTR.
i. The reactor’s residence time is defined as the reactor volume divided by the total feed flow
rates, F0. Calculate the average residence time, τavg.
V CSTR
Residence Time , τ=
F0
ii. Calculate the reaction rate constant, k, and the rate of reaction, –r NaOH using the average
residence time, τavg.
C A 0−C A
Reactionrate constant , k= 2
τ avg C A
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
ii. Calculate the reaction rate constant, k, and the rate of reaction, –r NaOH using the average
residence time, τavg.
C A 0−C A
Reactionrate constant , k= 2
τ avg C A
2
Rate of reaction ,−r NaOH =k C A
CA = The outlet concentration of NaOH (M) in the Table with the highest conversion, X
CA0 = The inlet concentration of NaOH (M) in the Table with the highest conversion, X
iii. Calculate the the Damnköhler (Da) number. In the 3-stage CSTR in series, all equal volume
and same operating temperature, the Damnköhler (Da) number for a second order reaction in a
CSTR is defined as
Da=τ avg k C A 0
7. Calculate the following parameter for the PFR
i. Calculate the reaction rate constant, k, and the rate of reaction, –rNaOH
( )
F 0 , avg X
Reaction rate constant , k=
V PFR C A 0 1− X
2
Rate of reaction ,−r NaOH =k C A
F0,avg = Average total inlet flow rate of solutions (mL/min)
CA0 = The inlet concentration of NaOH (M) in the Table with the highest conversion, X
CA = The outlet concentration of NaOH (M) in the Table with the highest conversion, X
X = The highest conversion in the Table
DISCUSSION
1. Discuss experimental work.
2. Examine the relationship between the plot conversion, X vs reaction time, t of the various types of
reactors. Discuss which configurations are best for this reaction based on the experimental results
and explain why.
3. Compare and discuss the reaction rate constant, k, and the rate of reaction, –r A for the various
types of reactors.
4. Examine the calculated Damnköhler (Da) number for the 3-stage CSTR’s in series and discuss its
correlation to the highest conversion achieved in this experiment.
TUTORIAL
1. State the differences between the three types of reactors: Single CSTR, 3-stages CSTR and PFR
reactor. Discuss the benefits and drawbacks of each configuration.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
2. Write a one-paragraph summary of any journal article on multiple stages CSTR reaction. The
article must be published within 202-2021. Explain the multiple stages CSTR used in the study
and its significance.
REFERENCES
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA), 1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall (USA), 1999.
3. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore), 1981.
4. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Use the calibration curve to determine the concentration of NaOH in the experiment.
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (FEB 2023) REACTION ENGINEERING (CKB 20104)
Total flow
Inlet Outlet
rate of
Flow rate Flow rate Residence concentration Outlet concentration Conversion,
solutions, Inlet
Temperature of NaOH, of Et(Ac), time, τ (min) of NaOH, Conductivit of NaOH, X (%)
Time F0 (mL/min) conductivity
(°C) FNAOH FET (Self- CNaOH (M) y CNaOH (M) (Self-
(min) = FNAOH + FET (mS/cm)
(mL/min) (mL/min) calculate) (Calibration (mS/cm) (Calibration calculate)
(Self-
curve) curve)
calculate)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
F0,avg = τavg =
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