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Group 8 - Experiment 3 - Batch Liquid Reactor
Group 8 - Experiment 3 - Batch Liquid Reactor
Group 8 - Experiment 3 - Batch Liquid Reactor
GROUP 8
NAME STUDENT ID
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CEB 2072 CHEMICAL ENGINEERING LAB II
TABLE OF CONTENT
TOPIC PAGE
CHAPTER 1: INTRODUCTION
1.2 Objectives 4
CHAPTER 2: METHODOLOGY
CHAPTER 4: CONCLUSION 21
CHAPTER 5: REFERENCES 22
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CHAPTER 1: INTRODUCTION
1.1 BACKGROUND STUDY
Reactors provide a means for forming raw materials into desired products under chemical
change, which is a crucial part of most industrial chemical processes. Batch reactors are widely
used in process industries and are preferred in laboratories and pharmaceutical plants. A batch
reactor has an agitator and a heat transfer coil. There are several advantages that a batch reactor
has over other reactors in such industries. Since batch reactors are simple to operate and allow
for simultaneous testing of multiple parameters, they are perfect for labs. In addition, batch
reactors are mainly used for relatively slow reactions that need a long period of time to
complete.
A batch reactor is commonly used for smaller operations such as testing new chemicals or
for processes that are difficult to convert into continuous ones (Fogler, 2006). Batch reactors
also offer higher conversion per unit volume than other reactors (Ahmad et al., 2013). Typically,
batch reactors are operated with constant volume and are operated isothermally. Thus, the
interpretation of results is easier since there is little auxiliary equipment required. Ethyl Acetate
and Sodium Hydroxide were used in this experiment to study and analyze the saponification
reaction and to prepare a conversion versus conductivity calibration curve. Free hydroxide ions
break esters between fatty acids and glycerol of triglycerides during saponification, resulting
in free fatty acids and glycerol. Alkaline conditions are required for saponification (Bursalt,
Ertunc & Akay,2006). There are many applications for sodium ethanol, a product of the
saponification process. In the textile industry, it is used to remove insoluble calcium salts, and
in the paint industry to enhance colors. In this process, the liquid phase is homogeneous, so
batch reactors are ideal (Abdalla Ahmed, 2015).
A batch reactor does not have either a feed stream and an exit stream. Therefore, the rate
of reaction is defined as:
1 dNA
rA =A dt
where V is the unit volume, dt is the unit time and dNA is the moles of A which appears by the
reaction. From this equation, we can conclude that if A is the reaction product, the rate becomes
positive whereas if A is the consumed reactant, the rate is negative.
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1.2 OBJECTIVES
• To prepare a calibration curve for conversion versus conductivity.
• To study the batch saponification reaction between Ethyl Acetate and Sodium Hydroxide
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CHAPTER 2: METHODOLOGY
2.1 MATERIAL AND APPRATUS
MATERIAL
No Material
1 Sodium Hydroxide (NaOH)
2 Sodium Acetate
3 Ethyl Acetate
4 Distillation water
5 Hydrochloric Acid (HCl)
APPRATUS
No Equipment Description
• A reactor consists of a
glass vessel with top and
bottom plate made of
stainless steel.
• The reactor is vacuum
1 Batch liquid reactor insulated by an outer
glass jacket.
• The reactor comes with a
cooling coil, a 1.0 kW
heater, a temperature
sensor and stirrer system.
• For each liquid reactant,
a 20-L feed tank, a pump,
a needle valve, and a
2 Feed tank system
flow meter are provided.
• Each reactant is pumped
from the feed tank to the
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Solutions
1-L of 0.05M NaO
1-L of 0.075M NaOH + 1-L of 0.025M Sodium Acetate
1-L of 0.05M NaOH + 1-L of 0.05M Sodium Acetate
1-L of 0.025M NaOH + 1-L of 0.075M Sodium Acetate
1-L of 0.05M Sodium Acetate
2. To start the experimental procedure, the main switch, Pump P1 and Pump P2 were switched
on to let the feed enter into the reactor.
3. After the glass reactor was filled until 2 litres volume, the Pump P1 and Pump P2 were
switched off.
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4. Then, the stirrer switch was turned on and it was set to 50rpm stirring speed.
5. The values of the conductivity values are recorded at 60 seconds interval in a table.12
readings were recorded in the table.
6. After the readings are obtained, the reactor is drained and flushed using deionized water.
7. Steps (2) till (5) were repeated with different solutions that had been prepared earlier.
8. The conductivity values for each of the stated solutions were recorded in the table below.
Conversion Conductivity
Solutions
[%] [mS/cm]
0.00 1-L of 0.05M NaOH 20.08
1-L of 0.075M NaOH + 1-L of 0.025M Sodium
0.25 14.73
Acetate
1-L of 0.05M NaOH + 1-L of 0.05M Sodium
0.50 11.32
Acetate
1-L of 0.025M NaOH + 1-L of 0.075M Sodium
0.75 9.03
Acetate
1.00 1-L of 0.05M Sodium Acetate 7.89
9. The slope and y-axis intercept from the plot of conversion vs conductivity was determined.
Reactants Preparation
1. 1 litre of 0.25 M standard HCl and 1 litre of 0.1 M standard NaOH were prepared.
2. 0.1 M NaOH solution was prepared in feed tank T1 and 0.1 M Ethyl acetate in feed tank
T2.
3. The concentration of our 0.1 M NaOH solution was confirmed by titrating a small amount
of it with standard 0.25 M HCl using phenolphthalein as indicator.
4. The concentration of the ethyl acetate solution was ensured using the following procedure:
5. First, 0.1 M NaOH solution was added to a sample of ethyl acetate solution such that the
0.1 M NaOH solution is in excess to ensure all of the ethyl acetate reacted. This mixture
was let to react overnight. Then, the amount of unreacted NaOH was determined by direct
titration with standard 0.25 M HCl. The ethyl acetate real concentration was recorded.
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y = -12.032x + 18.626
R² = 0.9323
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10
0
0 0.2 0.4 0.6 0.8 1 1.2
Conversion (%)
In this sub-experiment, sodium hydroxide (NaOH) and ethyl acetate are saponified to
create sodium acetate in a liquid batch reactor. The liquid batch reactor's saponification process
is used to study the connection between conductivity and conversion. Five solutions with
varying sodium hydroxide and sodium acetate concentrations are displayed on a calibration
curve. The graph is clearly depicted as descending linearly in Figure 3A.1 because to the R2
square value of 0.9323, which is very close to 1. The graph's y-intercept is 18.626 mS/cm,
while the slope is -12.032 mS/cm. Because the calibration curve has a negative slope, it can be
demonstrated that the conductivity is inversely proportional to the conversion. This is due to
the fact that when sodium hydroxide is converted into more sodium acetate, the concentration
of hydroxide ions (OH-) in the solutions keeps dropping. In other words, when conversion rises,
fewer hydroxide ions (OH-) are present in the solutions, which lowers their concentration and
lowers the concentration of OH- throughout the experiment, lowering conductivity as well. The
calibration curve's linear equation is depicted as follows.
𝑦 = −12.032𝑥 + 18.626
Where,
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For experiment B, the batch saponification reaction of ethyl acetate and sodium
hydroxide has been executed. Based on the calibration curve that was plotted in experiment A,
we use the linear equation order to find the value of the conversion. The value of conductivity
is given in the lab manual and the equation to find the conversion is below:
y= -12.032x + 18.626
After determining the value of conversion, we used the initial concentration of sodium
hydroxide (NaOH), CAo, of 0.1M to compute the value of concentration, CA. Furthermore, the
0th, 1st, and 2nd order graphs were plotted using the integral method. Using the method, we
can determine the kind of order depending on the graph's best linear fit. The graph will display
CA vs time for the 0th order, ln (CAo/CA) vs. time for the 1st order, and 1/CA vs time for the 2nd
order. The outcomes and discussions for each stirrer speed 50, 100, 150, and 200 rpm are listed
in the appendix.
a) 200rpm
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Three graphs have been plotted for 200 rpm stirrer speed. Based on the three graphs
(Figure 3.1B,figure 3.2B,figure 3.3B) , for zero order, the graph CA vs time has an inverse
trendline with the value of R2 of 0.9001 Next, for first order graph which is ln CAO/CA vs time,
the graph also has a decreasing but more more stable trendline with the value of R 2 of 0.9106.
Lastly, for second order graph which is 1/CA vs. time, the graph has an increasing trendline
with the value of R 2 of 0.9356.
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Based on theory, if the value of R2 is large or close to 1, the graph is considered having
a perfect fit. At the same time, it relates to the type of order we would like to determine as the
highest value of R2 will be chosen as the type of order. Based on the three graphs plotted for
200 rpm stirrer speed, it is observed that all three graph have different R2 value. The closest
value of R2 to 1 is the second order graph which have 0.9356 value of R2 . Therefore, the type
of reaction will be the second order.
After determining the type of order, which is second order, we can find the rate constant
value, k by taking it from the graphs that we have plotted. The slope of the second order graph
indicates the value of rate constant, k. Thus, the value obtained from the graph is 0.674 dm𝟑
mol x min.
b) 150rpm
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For 150 rpm stirrer speed, three graphs have been plotted (Figure 3.4B, Figure 3.5B,
Figure 3.6B). Based on the three graphs, for zero order, the graph CA vs time has a decreasing
trendline with the value of R2 of 0.7381. Next, for first order graph which is ln CAO/CA vs. time,
the graph also has an decreasing trendline with more stable with the value of R2 of 0.7819.
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Lastly, for second order graph which is 1/CA vs. time, the graph has an increasing trendline
with the value of R2 of 0.9696.
Based on theory, if the value of R2 is large or close to 1, the graph is considered having
a perfect fit. At the same time, it relates to the type of order we would like to determine as the
highest value of R2 will be chosen as the type of order. Based on the three graphs plotted for
150 rpm stirrer speed, the second order has the highest R2 value and we can conclude that it is
second order reaction.
After determining the type of order, which is second order, we can find the rate constant
value, k by taking it from the graphs that we have plotted. The slope of the second order graph
indicates the value of rate constant, k. Thus, the value obtained from the graph is 1.560 dm𝟑
mol x min.
c) 100rpm
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For 100 rpm stirrer speed, three graphs have been plotted (Figure 3.7B, Figure 3.8B,
Figure 3.9B). Based on the three graphs, for zero order, the graph CA vs time has a decreasing
trendline with the value of R2 of –0.006. Next, for first order graph which is ln CAO/CA vs time,
the graph also has an decreasing trendline with the value of R2 of 0.8676. Lastly, for second
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order graph which is 1/CA vs time, the graph has an increasing trendline with the value of R2
of 0.9818.
Based on theory, if the value of R2 is large or close to 1, the graph is considered having
a perfect fit. At the same time, it relates to the type of order we would like to determine as the
highest value of R2 will be chosen as the type of order. Based on the three graphs plotted for
100 rpm stirrer speed, the second order has the highest R2 value which is 0.9818 and it is the
closest to 1. therefore, we can conclude that it is second order reaction.
After determining the type of order, which is second order, we can find the rate constant
value, k by taking it from the graphs that we have plotted. The slope of the second order graph
indicates the value of rate constant, k. Thus, the value obtained from the graph is 1.4522 dm𝟑
mol x min.
d) 50rpm
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For 50 rpm stirrer speed, three graphs have been plotted (Figure 3.10B, Figure 3.11B,
Figure 3.12B). Based on the three graphs, for zero order, the graph CA vs time has a decreasing
trendline with the value of R2 of 0.8858. Next, for first order graph which is ln CAO/CA vs. time,
the graph also has an decreasing trendline with the value of R2 of 0.9057. Lastly, for second
order graph which is 1/CA vs time, the graph has an increasing trendline with the value of R2
of 0.9917.
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Based on theory, if the value of R2 is large or close to 1, the graph is considered having
a perfect fit. At the same time, it relates to the type of order we would like to determine as the
highest value of R2 will be chosen as the type of order. Based on the three graphs plotted for
100 rpm stirrer speed, the second order has the highest R2 value which is 0.9917 and it is the
closest to 1. therefore, we can conclude that it is second order reaction.
After determining the type of order, which is second order, we can find the rate constant
value, k by taking it from the graphs that we have plotted. The slope of the second order graph
indicates the value of rate constant, k. Thus, the value obtained from the graph is 1.1302 dm𝟑
mol x min .
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CHAPTER 4: CONCLUSIONS
This experiment is split into two parts. At the first stage, the calibration curve for the
graph of conversion against conductivity must be prepared. Sodium hydroxide and ethyl acetate
are saponified in a batch process in the second stage. The first stage is carried out with the same
stirrer speed and different amounts of Sodium Hydroxide and Ethyl Acetate. The derived
equation on the graph, y=-12.032x + 18.626, shows that the graph proves an increasing trend
for conversion but a decreasing trend for conductivity. Thus, conversion is inversely
proportional to the conductivity. The low concentration of NaOH, a strong base, creates
hydroxide ions, thus resulting into a reduced conductivity value and a poor capacity to transmit
electricity.
Before getting deeper into part B, there is a big chance that our result might differ from
the results from different groups. The reason behind this is because the accuracy of ethyl acetate
and sodium hydroxide mass could differ. The error can be avoided by properly locate the
chemicals into the container without spilling it around the container. For part B, we are
investigating the relationship between the sped of stirrer (200, 150, 100, 50) RPM and the
conductivity. As we can see in the graphs, all graphs following the best fit line is second order,
as shown by maximum R2 values that are near to 1, thus indicating the trend of the graph to be
upward. So, we can conclude that the higher the speed of the stirrer (RPM), the higher the
conductivity. This means that the speed of the stirrer and conductivity is directly proportional.
The reason behind this is because when the solution moves in a higher speed, the particles in
the solution will have higher chances to collide with other particles thus create friction. Since
we know that the friction is a type of energy (heat), thus the conductivity of the solution
increases.
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CHAPTER 5:REFERENCES
1. A comparative study of alkaline hydrolysis of ethyl acetate ... - IJCCE. (n.d.). Retrieved
February 15, 2023, from
https://www.ijcce.ac.ir/article_6743_b025a67f3916fddf87907acef52c9741.pdf
2. Ahmed, A. M. A. (n.d.). Saponification: A comparative kinetic study in a batch reactor.
CORE. Retrieved February 15, 2023, from https://core.ac.uk/outputs/71675705
3. Author links open overlay panelNihal Bursali a, a, b, AbstractThe purpose of this study
was to determine the effective operating parameters and the optimum operating conditions
of a batch saponification process in the frame of the process improvement. Full two-level
factorial and face-centered central compos, Montgomery, D. C., Carr, J. M., Lind, E. E.,
Xu, C.-P., & Anderson, M. J. (2006, March 30). Process Improvement Approach to the
saponification reaction by using statistical experimental design. Chemical Engineering and
Processing: Process Intensification. Retrieved February 21, 2023, from
https://www.sciencedirect.com/science/article/abs/pii/S0255270106000730
4. Comparative study of alkaline hydrolysis of ethyl acetate using ... - IJCCE. (n.d.). Retrieved
February 20, 2023, from
https://www.ijcce.ac.ir/article_6743_b025a67f3916fddf87907acef52c9741.pdf
5. Fogler, H. S. (n.d.). Elements of chemical reaction engineering. Google Books. Retrieved
February 21, 2023, from
https://books.google.com/books/about/Elements_of_Chemical_Reaction_Engineerin.html
?id=xuHFGWkuxJsC
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CHAPTER 6: APPENDIX
Part A: Calibration curve for Conversion vs Conductivity
Conductivity Conversion (X)
20.08 0
14.73 0.25
11.32 0.5
9.03 0.75
7.89 1
Table of the data for Conductivity and Conversion
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y = -12.032x + 18.626
R² = 0.9323
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10
0
0 0.2 0.4 0.6 0.8 1 1.2
Conversion (%)
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