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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

LABORATORY REPORT GUIDELINES

Each experimental report should contain the following items in accordance to the numbering as
listed:
1. COVER PAGE
Please insert the LABORATORY REPORT SUBMISSION FORM as the front cover.
DOWNLOAD FROM E-LEARNING.

2. TABLE OF CONTENTS
The table of content and number of pages should be in following format.
Note: Each page should be numbered.
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
Give the summary (not more than half page) on the overall experimental report. Give brief
review on the objectives of the experiment, main experimental results and discussions
which are deemed significant and finally conclusions obtained from the work.

4. RESULTS AND DISCUSSIONS


Note: Refer to the respective experimental procedure (Analysis and Discussion
sections) to determine the extent of analysis and discussions required.
a. Record down and present each of the experimental data and findings in proper manner.
b. Present the data either in Table, Graph, Histogram or Pie chart form as deemed suitable
with complete label and units.
c. Explanations of the referred table and figure must be presented below the table and
figure.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Example Table:
Table 1: X vs. Y
Samples X (unit) Y (unit)
A
B
C
D

Example Graph:
2.0
1.8
1.6
1.4
Parameter Y (unit)

1.2
1.0
0.8
y = -0.7886x + 1.7986
0.6
0.4
0.2
0.0
0.0 0.5 1.0 1.5
Parameter X (unit)

Figure 1: Relationship between X and Y

d. Based on the experimental results, discuss on your findings and relate to your theory
and objective of experiment

7. CONCLUSIONS AND RECOMMENDATIONS


a. Summary of the results to relate briefly the findings or results with the theory applicable
to the experimental
b. Suggest improvements in apparatus or measurement procedure, or even experimental
procedures for future work (if applicable).
c. Should be in one paragraph.

8. TUTORIAL
Tutorial are the questions as given in the laboratory procedures. All questions must be
answered as required or else marks would not be rewarded for this section.

9. REFERENCES
Details of published sources of material referred to or quoted in the text (including any
lecture notes and URL addresses of any websites used).

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
REFERENCES SHOULD BE IN COMPLETE FORM AS GIVEN BELOW OR ELSE MARKS
WILL BE DEDUCTED FOR EACH ERROR.
A. The references should be in following format:
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.
B. The references should be arranged according to the author name in alphabetical order.

10. APPENDICES
All the raw data and sample of calculations should be included here.
Note: students are given option to handwrite the calculations part as tasked in the report.
However, the other part of the report should be typed.

IMPORTANT NOTE:
1. Laboratory reports are meant to be group tasks.
2. Each member of the group is required to choose 1 part of each section to be executed
individually. Therefore, any information copied from another group or taken directly from other
sources such as Internet without proper references will not be tolerated and the report will be
marked as zero.
3. Laboratory report should be submitted directly to the lecturer in charge for date verification.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX
CHEMICAL PREPARATION

1. Ethyl acetate (CH3COOCH2CH3) (Liquid Phase)


Volume of ethyl acetate needed, V1 (L) from the original solution
æ mol ö
M2 ç ÷V2 (L)
è L ø
V1 (L) =
æ mol ö
10.10 ç ÷
è L ø
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

2. Sodium Hydroxide (NaOH) (Solid Phase)

Weight of NaOH required for experiment, mNaoH

æ mol ö æ g ö
mNaOH (g) = M 2 ç ÷ ´ MWNaOH ç ÷ ´V2 (L)
è L ø è mol ø
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, MW NaOH = 40.0 g/mol

3. Hydrochloric acid (HCl) (Liquid Phase)


Volume of hydrochloric acid needed, V1 (L) from the original solution
æ mol ö
M2 ç ÷V2 (L)
è L ø
V1 (L) =
æ mol ö
1.0 ç ÷
è L ø
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 (JAN 2019) REACTION ENGINEERING (CKB 20104)

LABORATORY MANUAL
REACTION ENGINEERING
CKB 20104

SEPTEMBER 2015

LIST OF EXPERIMENTS:

EXPERIMENT 1: BATCH REACTOR


Experiment A: The Batch Saponification of Ethyl Acetate
Experiment B: Effect of Temperature on the Batch Saponification
Reaction

EXPERIMENT 2: CONTINUOUS STIRRED TANK REACTOR (CSTR)


Experiment A: Effect of RTD on the Reaction in a CSTR
Experiment B: The Effect of Temperature on the Reaction in a CSTR

EXPERIMENT 3: PLUG FLOW REACTOR (PFR)


Experiment A: Effect of Residence Time on the Reaction in a PFR
Experiment B: Effect of Temperature on the Reaction in a PFR

EXPERIMENT 4: REACTOR TEST RIG (RTR)


Experiment A: Reactor Comparison Test

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT 1
BATCH REACTOR

OBJECTIVES
To measure the rate constant of the reaction between ethyl acetate and sodium hydroxide
under batch condition.
To study the liquid phase reaction kinetics in a batch reactor.
To study the effect of temperature on the reaction in a batch reactor.

Keywords: Batch reactor; Kinetics; Saponification reaction; Activation energy

1.0 GENERAL DESCRIPTION

1.1 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)

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
 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)

Figure 1: Batch Reactor Unit

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 some time 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:

CH 3 COOC2 H 5  OH   CH 3 COO  C 2 H 5 OH
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 analyzing samples from the reaction mixture every few minutes. The second order rate
constant is determined in two different ways:

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
a) Integrated rate law method

Assuming the reaction to be a simple, irreversible, second order process, then the rate law
for a batch process may be written

d [ ester ]
= k [ ester ] [OH ]
-
Rate = -
dt
Suppose that the concentrations of the ester and hydroxide are equal at the start of the
experiment and equal to CA0 mol/dm3, and that at some time t later, both the ester and
hydroxide concentration have fallen to CA. Therefore, we obtain

dCA
- = k [ ester ] éëOH - ùû = kCA2
dt
Separating the variables and integrating with appropriate boundary conditions,

CA t
dC A
ò = k ò dt Þ
1 1
- = kt
C A0 C A2 0 C A C A0

A plot of 1/CA against t should give a straight line with the gradient, k.

b) Half-life method

1 1 1 æ CA0 - CA ö
From - = kt can be rearranged to give k = ç ÷
CA CA 0 t è CACA0 ø

Let t1/2 be the time taken for the concentration of ester to be halved, C A  C A0 / 2 , then

1
k=
t1/2CA0
The time taken to halve the concentration of ester is inversely proportional to the initial
concentration. From plot of the ester concentration CA against t, it is possible to determine
t1 / 2 and hence the rate constant.

1.2 Safety Considerations


1. Students must not carry out laboratory work without the supervision of a lecturer.
2. Read operating instructions carefully, and make sure that you fully understand all
aspects of operation of the batch reactor unit.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
3. Safety glasses must be worn at all times during these experiments – remember
you are in charge of all safety aspects.
4. For each experimental setting, allow 10 minutes for equilibrium conditions to be
established.
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.
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.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

Experiment A: The Batch Saponification of Ethyl Acetate


2.0 EXPERIMENTAL PROCEDURES

1. Prepare the following solutions:

a) 1 L of sodium hydroxide, NaOH (0.1 M)


b) 250 mL of ethyl acetate, Et(Ac) (0.1 M)
c) 250 mL of hydrochloric acid, HCl (0.1 M)

2. Pipette 200 mL of 0.1M ethyl acetate, Et(Ac) solution into a clean dry conical flask

3. Placed 200 mL of 0.1M sodium hydroxide (NaOH) into 500 ml beaker.

4. Label 11 clean conical flasks from 1 to 11 and pipette 20 mL of 0.1M hydrochloric acid,
HCl into each of them (Flask 1 to 11).

5. Place the mechanical stirrer in the sodium hydroxide (NaOH) solution.

6. Turn on the stirrer and quickly pour all of the ethyl acetate, Et (Ac) from the conical flask
into the NaOH beaker, starting the stopwatch at roughly the mid-point of addition.

7. After 5 minutes, withdraw by pipette 20 mL of the reacting mixture and pour into Flask 1,
noting the time at the mid-point of delivery.

8. Titrate the content of Flask 1 with 0.1M sodium hydroxide, NaOH using two or three
drops of phenolphthalein as indicator. The color of the indicator will change from
colorless (acidic) to pink (basic).

9. Stop the titration once the change of indicator color is observed. Determine the amount
of NaOH needed.

10. Withdraw further samples at 10 (Flask 2), 15 (Flask 3), 20 (Flask 4), 25 (Flask 5), 30
(Flask 6), 35 (Flask 7), 40 (Flask 8), 50 (Flask 9), 60 (Flask 10) and 70 (Flask 11)
minutes. Repeat step 7 to 9.

11. Record the results in Appendix A.

3.0 ANALYSIS AND DISCUSSIONS

Method of Calculations to determine concentration of NaOH

Let titre of NaOH as = Y mL

The number of moles of 0.1M NaOH used in the titration = Acid neutralized in titration

0.1(Y )
mol
= 1000

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

0.1(20)
We know the initial quantity of 0.1M acid = mol
1000
The amount of acid neutralized by sample = Moles of NaOH present in the sample

0.1(20 -Y )
mol
= 1000

Thus, NaOH concentration in 20 mL sample from the reactor = Ester concentration =

0.1 ( 20 -Y )
´ mol / mL
= 1000 20

1. Plot a graph conversion, X vs. reaction time and discuss it thoroughly.

2. Determine the rate constant, k using both methods and compare both values as
explained previously:

a. Integrated rate law method

1 1
- = kt
C A C A0

A plot of 1/CA against t should give a straight line with the gradient, k.

b. Half-life method

* In the half-life method, the initial concentrations (CA0) can be obtained straight
forward. From the graph (CA versus t) we can determined how long it takes for
that concentration to be halved (t1/2 = Reaction time when concentration = 1/2
CA0).

1
k=
t1/2CA0

4.0 TUTORIAL
1. Discuss why it is vital to conduct certain chemical reactions in bench scale up and
subsequently discuss its disadvantages.
2. Write a one-paragraph summary of any journal article that studies chemical reaction in
a batch reactor. The article must have been published within the last 5 years. Explain
on the batch reactor used in the study and its significance to the study done.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Experiment B: Effect of Temperature on the Batch Saponification Reaction

5.0 EXPERIMENTAL PROCEDURES

1. Prepare the following solutions:


a) 6 L of sodium hydroxide, NaOH (0.1 M)
b) 6 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.
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 value and temperature value 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.
16. Repeat the experiment (steps 1-8) for different reactor temperature by setting the
thermostat temperature to the desired temperature.
17. Perform the general shutdown procedures.

6.0 General Shutdown Procedures


1. Keep the cooling water valve V5 open to allow the cooling water to continue flowing.
2. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to room
temperature.
3. Switch off the stirrer M1.
4. Close cooling water valve V5. Open bottom valve V1 to drain any liquid from the unit.
5. Turn off the power for the control panel.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
7.0 ANALYSIS AND DISCUSSIONS
1. Use the sample table in Appendix C for data collection.

2. Find the concentration of NaOH in the reactor from the calibration curve. Subsequently
calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph Conversion, X vs time, t for the different temperature and subsequently
compare the conversions for the different temperature. Discuss it thoroughly and
include explanations on the effect of temperature onto the reaction.

4. For a second order reaction, the rate law is shown to be:

dC A dC A
ò = -k ò dt
CA t
-rA = - = kC A2 AND
dt C A0
C A2 0

1 1
Therefore = kt +
CA CA0
where CA0 is the initial concentration of reactant NaOH in the reactor (0.05 M).

5. For each temperature value, plot the graph of ‘1/CA’ vs time, t and evaluate the slope and
y-axis intercept.

6. Determine the rate constant, k from the slope value for different temperature values.
Examine the change in the rate constant.

7. Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.

æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314 J/mol.K)
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø

8. Calculate the saponification reaction’s activation energy, E a and frequency factor, A


from the slope and intercept values using the Arrhenius equation.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
8.0 TUTORIAL
1. Describe an example of industrial applications other than saponification that utilized
batch reactors in its process. Discuss the advantages and disadvantages of using batch
reactors in chemical reaction.
2. Write a one-paragraph summary of any journal article that studies chemical reaction in
a batch reactor. The article must have been published within the last 5 years. Explain
on the batch reactor used in the study and its significance to the study done.

9.0 REFERENCES
1. Atkins, P.W. ‘Physical Chemistry’ (various ed.)
2. Smith, J.M. ‘Chemical Engineering Kinetics ‘(3rd ed.), McGraw-Hill, 1981
3. Frost, A.A. & Pearson, R.G. ‘Kinetics and Mechanics’ (2nd ed.), Wiley, 1961
4. Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd edition, Prentice Hall Int.
Series, N.J. (USA), 1997.
5. Levenspiel, O., Chemical Reaction Engineering, 3rd edition, John Wiley and Sons, 1999
6. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
7. Model SOLTEC BP 141 Operating Manual, Solution Engineering Bhd, KL.

APPENDIX A
Table for Experiment A: The Batch Saponification of Ethyl Acetate

Concentration of
Amount of NaOH, Conversion,
Time Flask
NaOH titred CNaOH (M) X (%)
(min) Number
(mL) (From equation (Self calculate)
above)
5 1
10 2
15 3
20 4
25 5
30 6
35 7
40 8
50 9
60 10
70 11

NOTE:
1. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX B
Experiment B: Effect of Temperature on the Batch Saponification Reaction

TABLE OF CALIBRATION CURVE

Concentratio
Conductivity
n of NaOH
(mS/cm)
(M)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M)
from the pre-determined conductivity found during the experiment.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX C
Table for Experiment B: Effect of Temperature on the Batch Saponification
Reaction

Volume of NaOH = 3L
Volume of Et(Ac) = 3L
Temperature = _____ C

Concentration of Conversion,
Time Temperature Conductivity NaOH, CNaOH (M) X (%)
(min) (°C) (mS/cm) (From calibration (Self
curve) calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured
conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

Continue:

Table for Experiment B: Effect of Temperature on the Batch Saponification


Reaction

Volume of NaOH = 3L
Volume of Et(Ac) = 3L
Temperature = _____ C

Concentration of Conversion,
Temperatur
Time Conductivity NaOH, CNaOH (M) X (%)
e
(min) (mS/cm) (From calibration (Self
(°C)
curve) calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured
conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

END EXPERIMENT 1

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT 2
CONTINUOUS STIRRED TANK REACTOR (CSTR)
OBJECTIVES
To study liquid phase reaction kinetics in a CSTR
To determine the conversion at different residence time.
To study the effect of temperature on the reaction in CSTR.

Keywords: CSTR; residence time; Mixing; Saponification kinetics; Activation energy

1.0 GENERAL DESCRIPTION


1.1 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
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
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
 Max coolant pressure of 2 bar with allowable temperature difference of 150°C
6. Receiving vessel (B3)
 100 L rectangular tank
7. Instrumentation
 Flow measurement (FI-301, FI-302)
 Temperature measurement (TI-101)
 Conductivity measurement (QI-401)

1.2 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 (JAN 2019) REACTION ENGINEERING (CKB 20104)

Vent

V1 V6

Cooling
Water
B1 B2 W1 Cooling
Water
V13
HS
1

Q1
M 401

TI
101
V2 V7
FI FI
301 302

V5 V10 R1
V3 V8
V3

V11
V4 V9
P1 P2
M M V12
HS HS
2 3 B3 T1

Figure 2: Continuous Stirred Tank Reactor Unit

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

2.0 OPERATING PROCEDURES

2.1 General Start-up 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.

2.2 General Shutdown Procedures

1. Keep the cooling water valve V13 open to allow the cooling water to
continue flowing.

2. Switch off both pumps P1 and P2. Switch off the stirrer M1.

3. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool
down to room temperature.

4. Close cooling water valve V13.

5. Open valves V4, V9 and V12 to drain any liquid from the unit.

6. Turn off the power for the control panel.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

Experiment A: Effect of RTD on the Reaction in a CSTR


3.0 EXPERIMENTAL PROCEDURES

3.1 OBJECTIVES:
 To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
 To determine the effect of residence time on the extent of conversion.
 To determine the reaction rate constant.
3.2 PROCEDURES:
1. Perform the general start-up procedures.
2. Switch ON both pumps P1 and P2 simultaneously.
3. Open and adjust the valves V5 (Monitor at FI-301) and V10 (Monitor at FI-
302) to give a flow rate of about 200 mL/min. Both must be adjusted to
equal flow rate.
4. Let the reactor fill up with both solutions until it is just about to 1/2 full.
5. Switch ON the stirrer M1.
6. Adjust the valves V5 and V10 to give the desired flow rate. Make sure that
both flow rates are maintained the same.
7. Start monitoring the conductivity value at QI-401.
8. 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).
9. 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.
10. End the experiment when the conductivity values do not change
significantly over time.
11. Repeat the experiment (steps 6 to 10) for different residence times by
adjusting the feed flow rates of NaOH and Et(Ac).
12. Make sure that both flow rates are maintained the same.
13. Perform the general shut-down procedures.
4.0 ANALYSIS AND DISCUSSION:

1. Use the table for data collection at Appendix B.

2. Find the concentration of NaOH in the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in
Appendix.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

3. Plot a graph of conversion, X vs. reaction time, t for the different flow rate.
Discuss the graph.

4. The reactor’s residence time is defined as the reactor volume divided by the
average total feed flow rates.

VCSTR
Residence Time, t =
F0

Subsequently calculate the average residence time, τavg (NOTE: 1 FLOW RATE
PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).

5. Compare the highest conversion, X for the different average residence time, τavg
(NOTE: 1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
Compare the highest conversion, X at the different average residence time, τavg.
Discuss thoroughly and explain how residence time can influence the rate of
reaction.

6. For the different average reactor residence times, τavg (NOTE: 1 FLOW RATE
GIVES 1 AVERAGE RESIDENCE TIME), calculate the value of the reaction rate
constant, k and the rate of reaction, –rA.

Reaction rate constant, k =


(C A0
- CA ) AND Rate of reaction, - r = kC A2
t avg C 2
A
A

τavg = Average residence time from 1 flow rate (min)


CA = Exit concentration of reactant NaOH (M) (Note: Concentration of
NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at t = 0)

5.0 TUTORIAL

1. Discuss the advantages and disadvantages of using CSTR reactors in chemical


reaction. Describe an example of industrial applications that utilized CSTR
reactors in its process.

2. Write a one-paragraph summary of any journal article that studies chemical


reaction in a CSTR. The article must have been published within the last 5 years.
Explain on the CSTR reactor used in the study and its significance to the study
done.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT B: The Effect of Temperature on the Reaction in a CSTR

6.1 OBJECTIVES:
 To determine the effect of temperature on the extent of conversion.
 To determine the value of the reaction’s activation energy.

6.2 PROCEDURES:
1. Perform the general start-up procedures.
2. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
3. Open cooling water valve V13 and let the cooling water flow through the
condenser W1.
4. Switch on the thermostat T1 and set the water temperature to the desired
temperature.
5. Switch ON both pumps P1 and P2 simultaneously.
6. Open and adjust the valves V5 (Monitor at FI-301) and V10 (Monitor at FI-302) to
give a flow rate of about 200 mL/min. Both must be adjusted to equal flow rate.
7. Let the reactor fill up with both solutions until it is just about to 1/2 full.
8. Switch ON the stirrer M1.
9. Start monitoring the conductivity value at QI-401.
10. Start the timer and record the conductivity value at QI-401, temperature value at
TI-101 and both flow rates (FI-301 and FI-302) when it has reached steady state
(Conductivity value begin to steadily decline with time).
11. Record the conductivity, temperature, both flow rate values for every 5 minutes
until the conductivity does not change over time. This is to ensure that the reactor
has reached steady state.
12. End the experiment when the conductivity values do not change significantly over
time.
13. Repeat the experiment (steps 6 to 11) for different reactor temperatures by setting
the thermostat temperature to the desired temperature. Make sure that the flow
rates of both solutions are maintained at the original flow rate.
14. Perform the general shut-down procedures.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

7.0 ANALYSIS AND DISCUSSION:


1. Use the sample table in Appendix B for data collection.

2. Find the concentration of NaOH in the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph of conversion, X vs. reaction time, t for the 2 different temperatures.

4. Compare the highest conversion, X at the different temperature. Discuss it


thoroughly and explain how temperature can influence the rate of reaction, –rA.

5. For different reactor temperatures, calculate the value of the reaction rate
constant, k.

Reaction rate constant,k =


(C A0
- CA )
t avg C 2
A

τ = Average residence time from 1 flow rate (min)


CA = Exit concentration of reactant NaOH (M) (Note:
Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)

6. Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.

æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314 J/mol.K)
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø

6. Calculate the saponification reaction’s activation energy, E a and frequency factor,


A from the slope and intercept values using the Arrhenius equation.

8.0 TUTORIAL
1. Discuss the advantages and disadvantages of using CSTR reactors in chemical
reaction. Describe an example of industrial applications that utilized CSTR
reactors in its process.
2. Write a one-paragraph summary of any journal article that studies chemical
reaction in a CSTR. The article must have been published within the last 5 years.
Explain on the CSTR reactor used in the study and its significance to the study
done.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

9.0 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.

APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentratio
Conductivity
n of NaOH
(mS/cm)
(M)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-
axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product
(M) from the pre-determined conductivity found during the experiment.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

APPENDIX B
RESULTS FOR EXPERIMENTS

Reactor volume= 10 L Flowrate = _____ mL/min


Temperature = _____ oC

Total flow rate Concentration


Residence
Flow rate of Flow rate of of solutions, time, τ
of NaOH, Conversion,
Temperatur F0 (mL/min), Conductivity CNaOH (M) X (%)
Time NaOH, FNAOH Et(Ac), FEt (min)
e (°C) = FNAOH + FEt (mS/cm) (From (Self–
(mL/min) (mL/min) (Self–
(Self– calibration calculation)
calculation)
calculation) curve)
0
5
10
15
20
25
30
35
40
45
50
55
60
τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS

Reactor volume= 10 L Flowrate = _____ mL/min


Temperature = _____ oC

Total flow rate Concentration


Residence
Flow rate of Flow rate of of solutions, time, τ
of NaOH, Conversion,
Temperatur F0 (mL/min), Conductivity CNaOH (M) X (%)
Time NaOH, FNAOH Et(Ac), FEt (min)
e (°C) = FNAOH + FEt (mS/cm) (From (Self–
(mL/min) (mL/min) (Self–
(Self– calibration calculation)
calculation)
calculation) curve)
0
5
10
15
20
25
30
35
40
45
50
55
60
τavg =
NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT

PLUG FLOW REACTOR (PFR)


OBJECTIVES
To determine the effect of residence time on the conversion in a PFR.
To determine the effect of temperature on the conversion in a PFR.

Keywords: PFR, pulse input, step input, residence time

1.0 GENERAL DESCRIPTION


1.1 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.

1. Plug flow reactor (SR1)

 Jacketed pipe with approximate capacity of 1.5 L

 Pipe length 15 m

2. Feed vessels (B1/B2)

 60 L PE rectangular vessels with all necessary connections

2. Dosing vessels (HB1/HB2)

 1 L cylindrical vessels with overflow port and bottom port

3. Pumps (P1/P2)

 Centrifugal pumps

 Max delivery rate of 60 L/h and max delivery height of 8 m

4. Pre-heater (W1/W2)

 Coil heat exchanger, area 0.06 m2

 Max heating media pressure of 0.5 bar

5. Receiving vessel (B3)

 100 L rectangular tank

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

6. Instrumentations

 Flow measurements (FI-301, FI-302, FI-303)

 Temperature measurements (TI-101, TI-102)

 Conductivity measurements (QI-401, QI-402)

1.2 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 (JAN 2019) REACTION ENGINEERING (CKB 20104)

Vent

QI TI
402 102
V10
HB1 HB2

SR1

V1 V2 T1

W1 W2 TI QI
101 401

Injection

B1 B2 FI
301
FI
302
FI
303
B3
V11

V3 V4 V7 V8 V9
P1 P2
M M
V5 V6
HS HS Process Water
1 2
V12

Figure 3: Plug Flow Reactor Unit

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

2.0 OPERATING PROCEDURES

2.1 General Start-Up Procedures for Experiments A & B

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.

2.3 General Shut-Down Procedures

1. Switch off both pumps P1 and P2.

2. Switch off the thermostat T1.

3. Close the process water valve V12.

4. Open valves V3, V4, V5, V6, V7, V8 and V11 to drain all liquid from the unit.

5. Turn off the power for the control panel.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT A: Effect of Residence Time on the Reaction in a PFR


3.0 EXPERIMENTAL PROCEDURES

3.1 OBJECTIVE

 To carry out a saponification reaction between NaOH and Et(Ac) in a PFR.


 To determine the reaction rate constant.
 To determine the effect of residence time on the conversion in a PFR.

3.2 PROCEDURES:
1. Perform the general start-up procedures
2. 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 400 mL/min. Make sure that
both flow rates are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor
SR1 and empty into the receiving vessel B3.
4. Adjust valves V7 and V8 to give the desired flow rate. Make sure that both
flow rates are the same.
5. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
6. 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).
7. 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.
8. Repeat the experiment (steps 4 to 5) for different residence times by
adjusting the flow rates to the desired values. Make sure that both flow
rates are the same.

4.0 ANALYSIS AND DISCUSSION:


1. Use the table for data collection at Appendix B.

2. Find the concentration of NaOH in the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in
Appendix.

3. Plot a graph of conversion, X vs. reaction time, t for the different flow rate.
Discuss the graph.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

4. The reactor’s residence time is defined as the reactor volume divided by the
average total feed flow rates.

VPFR
Residence Time, t =
F0

Subsequently calculate the average residence time, τavg (NOTE: 1 FLOW RATE
PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).

5. Compare the highest conversion, X for the different average residence time, τavg
(NOTE: 1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
Compare the highest conversion, X at the different average residence time, τavg.
Discuss thoroughly and explain how residence time can influence the rate of
reaction.

6. For the different average reactor residence times, τavg (NOTE: 1 FLOW RATE
GIVES 1 AVERAGE RESIDENCE TIME), calculate the value of the reaction rate
constant, k and the rate of reaction, –rA.

F0,avg æ X ö
Reaction rate constant, k = ç ÷ AND Rate of reaction, - rA = kC A
2

VPFRC A0 è 1- X ø

F0, avg = Average total inlet flow rate of solutions (mL/min)


CA= Exit concentration of reactant NaOH (M) (Note: Concentration of NaOH at
the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at t=0)
X = Conversion (NOTE: Choose Highest Conversion X)

5.0 TUTORIAL

1. Discuss the advantages and disadvantages of using PFR reactors in chemical


reaction. Describe an example of industrial applications that utilized PFR
reactors in its process.

2. Write a one-paragraph summary of any journal article that studies chemical


reaction in a PFR. The article must have been published within the last 5 years.
Explain on the PFR reactor used in the study and its significance to the study
done.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT B Effect of Temperature on the Reaction in a PFR

6.1 OBJECTIVE:

 To determine the effect of temperature on the conversion in a PFR.

6.2 PROCEDURES:

1. Perform the general start-up procedures.

2. Check that there is sufficient water in the thermostat T1 tank. Refill as


necessary.

3. Open the process water valve V12.

4. Switch on the thermostat T1 and set the water to the desired temperature.

5. 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 400 mL/min. Make sure that
both flow rates are the same.

6. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor
SR1 and empty into the receiving vessel B3.

7. Adjust valves V7 and V8 to give a flow rate of about 100 mL/min. Make sure
that both flow rates are the same.

8. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).

9. Start the timer and record both conductivity values (QI-401 and QI-402) flow
rates (FI-301 and FI-302), and temperatures ((TI-101 and TI-102) when it
has reached steady state (Conductivity value begin to steadily decline with
time).

10. Record the conductivity, flow rates, and temperatures for every 5 minutes
until they do not change over time. This is to ensure that the reactor has
reached steady state.

11. Repeat the experiment (steps 5 onwards) for different reactor temperatures
by increasing the thermostat temperature to the desired temperature. Make
sure that the flow rates of both solutions are maintained at 100 mL/min.

7.0 ANALYSIS AND DISCUSSION

1. Use the sample table in Appendix B for data collection.

16
LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

2. Find the concentration of NaOH in the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph of conversion, X vs. reaction time, t for the 2 different temperatures.

4. Compare the highest conversion, X at the different temperature. Discuss it


thoroughly and explain how temperature can influence the rate of reaction, –rA.

5. For different reactor temperature, calculate the value of the reaction rate constant,
k.

F0,avg æ X ö
Reaction rate constant, k = ç ÷
VPFRC A0 è 1- X ø

F0 = Average total inlet flow rate of solutions (mL/min)


CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)
X = Conversion (NOTE: Choose Highest Conversion X)

6. Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.

æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø
J/mol.K)

7. Calculate the saponification reaction’s activation energy, E a and frequency factor,


A from the slope and intercept values using the Arrhenius equation.

8.0 TUTORIAL

1. Discuss the advantages and disadvantages of using PFR reactors in chemical


reaction. Describe an example of industrial applications that utilized PFR reactors
in its process.

2. Write a one-paragraph summary of any journal article that studies chemical


reaction in a PFR. The article must have been published within the last 5 years.
Explain on the PFR reactor used in the study and its significance to the study
done.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

9.0 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

APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentratio
Conductivity
n of NaOH
(mS/cm)
(M)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-
axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product
(M) from the pre-determined conductivity found during the experiment.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS

Reactor volume = 1.5 L Flowrate = _____ mL/min


Temperature = _____ oC

Total flow Inlet Outlet


Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, n,
Temperature of NaOH, time, τ (min) conductivit Conductivit n of NaOH,
Time Et(Ac), F0 (mL/min) CNaOH (M) C (M) X (%)
(°C) FNAOH (Self- y NaOH
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS

Reactor volume = 1.5 L Flowrate = _____ mL/min


Temperature = _____ oC

Total flow Inlet Outlet


Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, n,
Temperature of NaOH, time, τ (min) conductivit Conductivit n of NaOH,
Time Et(Ac), F0 (mL/min) CNaOH (M) C (M) X (%)
(°C) FNAOH (Self- y NaOH
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

EXPERIMENT 4
REACTOR TEST RIG
OBJECTIVES
To compare the performance of single reactor, 3 CSTRs AND PFR.

Keywords: CSTR, PFR, Reactors in series; Conversion; Residence time distribution (RTD) studies

1.0 GENERAL DESCRIPTION

1.1 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)


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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

 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)

1.2 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 (JAN 2019) REACTION ENGINEERING (CKB 20104)

Vent

V22 V23 V24 M2 V25


HS
4
QI
404
M M3
HS
TI
5
104

M M4
HB1 HB2 HS T1
6
TI
103
M
QI
403
R2
M1 V16
HS
3 R3
TI

V1 V2
102 V17
M
QI
402 R4
SR1
W1 W2 V18

V11 V12 V13

QI TI
401 101 R1
V14
Injection
V15
FI FI FI
B1 B2 301 302 303

V19 V20 V21


V8 V9 V10

P1 P2 V27
V3 V4
M M V5 V6 Process Water
HS HS
V7
1 2 B3 V26

Figure 4: Reactor Test Rig


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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

2.0 OPERATING PROCEDURES


2.1 General Start-Up Procedures for Experiment
1. Ensure that all valves are initially closed.
2. 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)
3. Fill the feed vessel B1 with the NaOH solution and feed vessel B2 with the Et(Ac)
solution.
4. Turn on the power for the control panel.
5. Open the process water valve V27.
6. Open valves V1 and V2.
7. Switch on both pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions
into the dosing vessels HB1 and HB2, towards valves V10 and V9 respectively.
8. Make sure that the pipelines before valves V9 and V10 are filled with liquid. Bleed
any trapped air in the pipelines by using valves V9 and V10.
9. Allow both solutions to overflow in the dosing vessels HB1 and HB2 into the feed
vessels B1 and B2 respectively.
10. The unit is now ready for experiment.
2.2 Selection of Reactors
Any one of the three reactors provided in the reactor test rig can be used for each of
the experiments. The following procedures will explain the steps needed to select a
particular reactor to run an experiment.
1. Ensure that all valves from V3 to V21 are closed.
2. For the plug flow reactor SR1:
a) Open valves V11 and V19.
b) Read the outlet conductivity value from QI-404 and temperature value from
TI-104.
3. For the single stage continuous stirred tank reactor R1:
a) Open valves V13 and V14.
b) Switch on the stirrer M1.
c) Read the outlet conductivity value from QI-402 and temperature value from
TI-102.
4. For the 3-stage continuous stirred tank reactors R2, R3 and R4:
a) Open valves V12 and V21.
b) Switch on the stirrers M2, M3 & M4.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

c) Read the outlet conductivity value from QI-403 and temperature value from
TI-103.
2.3 General 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.

3.0 EXPERIMENTAL PROCEDURES

3.1 OBJECTIVE:

 To carry out a saponification reaction between NaOH and Et(Ac) using


different types of reactors.
 To compare the reaction conversion between different types of reactors.
 To determine the reaction rate constant.

3.2 PROCEDURES:
1. Perform the general start-up procedures

Plug Flow Reactor, PFR


2. Open valves V11 and V19.
3. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
4. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-404).
7. Start the timer and record both conductivity values (QI-401 and QI-404) and
flow rates (FI-302 and FI-303) when it has reached steady state
(Conductivity value begin to steadily decline with time).
8. 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.
9. Repeat the experiment (steps 2 to 6) by selecting a different reactor.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

Single stage continuous stirred tank reactor


1. Open valves V13 and V14.
2. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
4. Switch on the stirrer M1.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
7. Start the timer and record both conductivity values (QI-401 and QI-402) and
flow rates (FI-302 and FI-303) when it has reached steady state
(Conductivity value begin to steadily decline with time).
8. 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.
9. Repeat the experiment (steps 2 to 6) by selecting a different reactor.

3-stage continuous stirred tank reactors


1. Open valves V12 and V21.
2. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
4. Switch on the stirrer M2, M3 and M4.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-403).
7. 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).
8. 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.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

4.0 ANALYSIS AND DISCUSSION:


1. Use the sample table in Appendix B for data collection.

2. Find the concentration of NaOH exiting the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph of conversion, X vs. reaction time for each of the reactor.

4. Compare the graphs between the different types of reactors and observe the
relationship. Based on the experimental results, discuss which configurations are
the best for this reaction and state the reasons accordingly.

5. Determine the following parameters:

a) Single stage CSTR

1. The reactor’s residence time is defined as the reactor volume divided by


the average total feed flow rates.

VCSTR
Residence Time, t =
F
0

Subsequently calculate the average residence time, τavg

2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

Reaction rate constant, k =


(C A0
- CA ) AND Rate of reaction, - r = kC A2
t avg C 2
A
A

τavg = Average residence time (min)


CA = Exit concentration of reactant NaOH (M)
(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)

b) 3-stage CSTR’s in series

1. The reactor’s residence time is defined as the reactor volume divided by


the average total feed flow rates.

VCSTR
Residence Time, t =
F
0

Subsequently calculate the average residence time, τavg


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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

Reaction rate constant, k =


(C A0
- CA ) AND Rate of reaction, - r = kC A2
t avg C 2
A
A

τavg = Average residence time (min)


CA = Exit concentration of reactant NaOH (M)
(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)

3. In the 3-stage CSTR in series, all of equal volume and same operating
temperature, the Damnköhler (Da) number for a second order reaction in
a CSTR is defined as, Da = τavgkCA0. Calculate the the Damnköhler (Da)
number and discuss its correlation to the highest conversion achieved in
this experiment.

c) Plug flow reactor (PFR)

1. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

F0,avg æ X ö
Reaction rate constant, k = ç ÷ AND Rate of reaction, - rA = kC A
2

VPFRC A0 è 1- X ø

CA = Exit concentration of reactant NaOH (M)


(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)
X = Extent of conversion (NOTE: Choose Highest Conversion X)
F0,avg = Average total inlet flow rate of solutions (mL/min)

5.0 TUTORIAL
1. Write the differences between 3 reactors: Single CSTR, 3-stages CSTR and
Tubular (PFR) reactor. Discuss the advantages and disadvantages for each
configuration.
2. Write a one-paragraph summary of any journal article that studies chemical
reaction in a multiple stages CSTR. The article must have been published within

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

the last 5 years. Explain on the PFR reactor used in the study and its significance
to the study done.

6.0 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.
APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentratio
Conductivity
n of NaOH
(mS/cm)
(M)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M)
from the pre-determined conductivity found during the experiment.

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = PFR Reactor volume = 3L

Total flow Inlet Outlet


Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, n of NaOH, n,
Temperature of NaOH,
Et(Ac), time, τ (min) conductivit Conductivit
Time (°C) FNAOH F 0 (mL/min)
(Self- CNaOH (M) y CNaOH (M) X (%)
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = Single-stage CSTR Reactor volume = 4L


Total flow Inlet Outlet
Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, n,
Temperature of NaOH, time, τ (min) conductivit Conductivit n of NaOH,
Time Et(Ac), F 0 (mL/min) CNaOH (M) CNaOH (M) X (%)
(°C) FNAOH (Self- y
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH

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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = 3-stage CSTRs Reactor volume = 1L

Total flow Inlet Outlet


Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, n,
Temperature of NaOH, time, τ (min) conductivit Conductivit n of NaOH,
Time Et(Ac), F0 (mL/min) CNaOH (M) C (M) X (%)
(°C) FNAOH (Self- y NaOH
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
39