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TABLE OF CONTENT
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1.0 ABSTRACT
The Continuous Stirred Tank Reactor (CSTR) experiment is to study the reaction between
Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac). This experiment is to identify the effect
of temperature and reaction rate. The CSTR experiment also to determine the relationship
between reaction rates on conversion, reactor volume and feed rate. During the experiment,
NaOH and Ethyl Acetate are mixed with equal volume for both by using CSTR at 40°C. First
50 mL of the sample solution is collected and undergo titration using 0.1M of NaOH. The
sample of solution is collected for every 5minutes consecutively. The amount of NaOH used
in titration are recorded. The solution in the CSTR is drained before another reaction of Ethyl
Acetate and NaOH are mix using different temperature which is 50°C and 60°C by using same
procedure. The result is recorded, calculation is made and graph is plotted based on the
results. Based on the graph plotted, the rate constant, k obtained is 0.8734 /mol.min and
0.3539 L/mol.min at 40oC and 50oC respectively. At both temperature has 2nd order of reaction.
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2.0 INTRODUCTION
In chemical industrial, it is widely essential for the reaction related to chemical kinetics and
reactor design. The secret to a chemical plant’s success or failure is the choice of the
reaction system that operates in the safest and most efficient way. Reactor is a device that
converts raw material into something we desired. A good reactor provide high output and
low cost. One of the requirements for constructing or choosing a reactor is acknowledge
the reactor’s own performance. Many reactors are depend on the nature of the feed
materials and products. We also need to know the rate reaction of the chemical reaction.
There are two type of reaction which are exothermic and endothermic in a reactor. To
maintain the reaction temperature in the reactor, a reactor is generally assembled with a
jacket or coil. When heat release due to exothermic reaction, there is a need for a coolant
flow to pass through the jacket or coil to absorb the heat released.
On the other hand, if there is endothermic reaction in the system, the hot stream moves
through the jacket or coil to maintain the temperature of the reaction. Meanwhile, if any
exothermic and endothermic reactions are involved in the reactor, the temperature of the
reaction varies with time for the non-isothermal reactor which an energy balance is needed.
There is no heat exchange between the process and the atmosphere in an adiabatic
reactor. Therefore, no medium is needed for heating or cooling. A chemical reactor is a
vessel where reaction is occur by conducting which is mean one or more chemical reaction
There is no heat exchange between the process and the atmosphere in adiabatic reactor.
Therefore no medium is needed for heating and cooling. A chemical reactor is a vessel
where reaction is carried out in order to produce product from reactant by means one or
more chemical reactions occurs. Depending the type of flow, a chemical reactor may be
characterized by the activity of the process. In this experiment, Continuous Stirred Tank
Reactor Model BP-100 is used.
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3.0 OBJECTIVES.
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4.0 THEORY
Continuous stirred tank reactor (CSTR) is a batch reactor equipped with stirrer or impeller that
provided efficient mixing. CSTR often used to refer an agitated tank reactor used to model
operation variables required to attain a specified output as having no spatial variations in
concentrations, temperature or reaction rate throughout the vessel. CSTR equipped with
features to continuously feed run with steady state and exhaust reactants in an example of
mechanically mixed flow reactor. Since in the CSTR has an identical in temperature and
concentration everywhere, the temperature and concentration of the exits point is same as the
temperature and concentration everywhere in the CSTR.
𝑑𝑁𝑎
- It is a steady-state, therefore 𝑑𝑡
=0
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- Rearranging the equation in terms of conversion:
As a function of the conversion –rA= f(x) which can size any type of reactor.
𝐹𝐴𝑜 1
This can be done by constructing a Levenspiel Plot which has function of or
−𝑟𝐴 −𝑟𝐴
𝐹𝐴
as X. While −𝑟 𝑜 vs X has volume of CSTR which is represented as a shaded area in
𝐴
As the temperature increases, the rate of reaction also increases. When the temperature is
increases by 10°C, the rate of reaction will be double. At a low temperature, the molecules
still collide each other unfortunately it is bounce apart. While, at high temperature, the bond
of the molecule will break and formed a new molecule. Based on collision theory, there are
some conditions must be occupied in order a reaction to occur, which are:
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- The molecule should have sufficient energy to break the energy barrier. Although
increasing temperature will increase the reaction, the molecules also should
overcome the energy barrier or minimum energy by another energy known as
activation energy (Ea) as shown in Arrhenius Law Equation:
𝐸𝑎
𝑘 = 𝐴𝑒 −𝑅𝑇
k = Rate constant
EA = Activation energy
R = Gas constant
T = Temperature (K)
A = Arrhenius factor
In this experiment, Residence Time Distribution (RTD) is used in order to provide information
about what is happening in the reactor. Residence time represents the average amount of
time for a mixture spends in a reactor. The data of residence time can be used to plot graph
concentration, C(t) versus time, t in order to observe the trends of the effluent tracer
concentrations. The data can be reduce to RTD function, E(t). The characteristic parameters
of the distribution function, E(t) such as mean residence time, variance of the distribution,𝜎
were deduced. Besides, the empirical E(t) parameter determined, theoretical RTD model
formula was applied to assess the corresponding theoretical RTD parameters such as
equivalent “n” via n-CSTR theoretical flow model and the axial dispersion coefficient using
axial dispersion model (Obonukut1, 2016).
Residence time also affected by the flowrate of a reactant entering the reactor. As the flowrate
increases, the residence time will decreases and the rate of reaction also decreases. Thus,
the residence time is directly proportional to the rate of reaction. Formula to calculate the
residence time is:
𝐶𝐴0 − 𝐶𝐴
𝜏=
−𝑟𝐴
𝜏 = Residence time
−𝑟𝐴 = Rate of reaction
CAo = Initial concentration
CA = Final concentration
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5.0 MATERIALS AND APPARATUS
5.1 MATERIALS.
1. 0.1 M Sodium Hydroxide, NaOH
2. 0.1 M Ethyl Acetate, Et(Ac)
3. 0.25 Hydrochloric Acid
4. Phenolphthalein.
5.2 APPARATUS.
1. Conical flask
2. 100mL measuring cylinder
3. 50 mL burette
Figure 3: Continuous Stirred Reactor unit BP-100.
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6.0 METHODOLOGY
1. P1 pump is switched on, 1.25 L of 0.05 M Ethyl Acetate, Et(Ac) is pumped from
feed tank to the reactor.
2. P2 is switched on, 1.25 L of 0.05M NaOH is pumped to the reactor. P2 is
stopped when the total volume reached 2.5 L.
3. The heater and stirrer are switched on and 30oC is set for the temperature and
timer is started.
4. After 5minutes of the reaction, 5 mL of the sample solution is collected from the
reactor. The sample is titrated with NaOH.
5. The sample is collected for the next 10, 15, 20 and 25 minutes for 5 mL.
6. The solution is drained, and the experiment is repeated using 40oC and 50oC.
7.0 Titration procedures.
1. 10 mL of 0.25M HCL is prepared in a conical flask.
2. 5 mL sample solution collected in experiment of CSTR is added into the conical
flask for the saponification reaction.
3. 3 drops of phenolphthalein act as indicator are added to the conical flask.
4. The mixture is titrated with 0.1 M NaOH until light pink colour is formed.
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5. The volume of NaOH used in the titration is recorded.
1. The cooling water valve from the main pipe is keep opened in order to allow
the cooling water to flow.
2. Pump P1 and P2 are switched off. The stirrer and heater are switched off to let
the equipment cooled down at the room temperature.
3. The cooling water valve from main pipe is closed.
4. Power control panel is closed.
5. The reactor tubing’s are cleaned properly to avoid corrosion of the equipment
due to the present of NaOH and Et(Ac).
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7.0 RESULTS
7.1 Effect of Residence Time.
Temperature at 29.9oC (room temperature):
Zeroth Order:
Figure 4: Graph CA versus Time
0.03
R² = 0.8122
0.02
0.015 CA
0.005
0
0 5 10 15 20 25 30
Time (min)
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First Order:
Figure 5: Graph Log CA versus Time
-0.4
-0.6
Log CA (mol/L)
-0.8
-1 Log CA
-1.2 Linear (Log CA)
y = -0.0119x - 1.5826
-1.4
R² = 0.8725
-1.6
-1.8
-2
Time (min)
Second Order:
Figure 6: Graph 1/ CA versus Time
50 y = 1.3775x + 38.342
R² = 0.9005
40
1/ CA
30
Linear (1/ CA)
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10
0
0 5 10 15 20 25 30
Time (min)
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Third Order:
Figure 7: Graph 1/CA2 versus Time.
5000
1/CA2 (L2/ mol2. min)
4000
3000
y = 149.09x + 1342.1 1/CA2
R² = 0.9562
2000 Linear (1/CA2)
1000
0
0 5 10 15 20 25 30
Time (min)
Based on figure 5, the slope of the graph is 1.3775. Thus, the rate constant, k at 29.9oC is
1.3775 L/mol.min at 2nd order.
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7.2 Effect of Temperature.
Temperature at 40oC:
Table 2: Data obtained at 40oC
Zeroth Order:
Figure 8: Graph CA versus Time
0.013
0.012 CA
0.011 Linear (CA)
0.01
0.009 y = -0.0001x + 0.0139
0.008 R² = 0.4501
0 5 10 15 20 25 30
Time (min)
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First Order:
Figure 9: Graph Log CA versus Time
-1.8
Log CA (mol/L)
-1.85
Log CA
-1.9 Linear (Log CA)
-1.95
y = -0.0047x - 1.8678
R² = 0.437
-2
Time (min)
Second Order:
Figure 10: Graph 1/CA versus Time
80 y = 0.8734x + 73.265
75 R² = 0.5347
1/CA
70
65 Linear (1/CA)
60
55
50
0 5 10 15 20 25 30
Time (min)
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Third Order:
Figure 11: Graph 1/CA2 versus Time
9000
1/CA2 (L2/ mol2.min)
8000
4000
3000
0 5 10 15 20 25 30
Time (min)
As shown in figure 10, from the graph plotted the slope id 0.8734. Hence, the rate constant
at temperature 40oC is 0.8734 L/mol.min at 2nd order.
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Temperature at 50o:
Table 3: Data obtained at temperature 50oC
Zero Order:
Figure12: Graph CA versus Time
0.032
0.03
CA
0.028
0.026 Linear (CA)
0.024 y = -0.0004x + 0.0353
0.022 R² = 0.6296
0.02
0 5 10 15 20 25 30
Time (min)
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First Order:
Figure 13: Graph Log/CA versus Time
-1.44
-1.46
Log CA (mol/ L)
-1.48
-1.5 y = -0.0049x - 1.4545 Log CA
-1.52 R² = 0.6585 Linear (Log CA)
-1.54
-1.56
-1.58
-1.6
Time (min)
Second Order:
Figure 14: Graph 1/ CA versus Time
32 y = 0.3539x + 28.606
30 R² = 0.6931
1/ CA
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26 Linear (1/ CA)
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22
20
0 5 10 15 20 25 30
Time (min)
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Third Order:
Figure 15: Graph 1/CA2 versus Time
1400
1/CA2 (L2/mol2.min)
1200
y = 22.195x + 826.22
1000 R² = 0.7258
1/ CA2
800 Linear (1/ CA2)
600
400
0 5 10 15 20 25 30
Time(min)
Based on figure 14, the slope from graph plotted at temperature 50oC is 0.3539. Thus, the
rate constant, k is 0.3539 L/mol.min at 2nd order.
ln k versus (1/T)
0
0.00305 0.0031 0.00315 0.0032
-0.2
y = 9040x - 28.973
ln k (L/mol.min)
-0.4 R² = 1
-0.6 Y-Values
Linear (Y-Values)
-0.8
-1
-1.2
1/T (K-1 )
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8.0 CALCULATION
Sample Calculation:
𝐶𝑁𝐴𝑂𝐻
V1= 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑
𝐶𝐻𝐶𝑙
0.1 𝑚𝑜𝑙/𝐿
V1= 𝑥 10.5 𝑚𝐿
0.25 𝑚𝑜𝑙/𝐿
V1= 4.20 mL
1 1
First order: = 𝑚𝑜𝑙
𝐶𝐴 0.029 𝐿
= 34.483 L/mol
1 1
Third order: =
𝐶𝐴2 0.029𝑚𝑜𝑙/𝐿
= 1189.061 L2/mol2.min
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Rate constant, k is obtained from the slope.
Rate of reaction, -rA= kCA2
= (1.3775) (0.0292)
=0.00116 L/mol.min
Activation energy, Ea :
o From figure 16, the linear line obtained from the graph is y = 9040x + 28.973.
o Based on the graph in figure 16 x-axis and y-axis, ln k= 9040(1/T) + 28.973
-Ea/R = 9040(K)
Ea = 9040(8.314)
Ea = -75158.56J/mol
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9.0 DISCUSSION
9.1 Effect of Residence Time
Residence time is a time period for a reactant stay in a reactor for a reaction occurs. The
longer the time for a reactant stay in the reactor the higher the reaction rate of the reactant.
This is because the longer the reactant stay in the reactor, it will decreases the
concentration of reactant as it exiting the reactor.
As shown in figure 4, as the time increases, the concentration of the reactant decreases.
At 29.9oC, the mixture of NaOH and Et(Ac) is enter the reactor. After a minute, the
concentration of mixture exit from the reactor contains 0.029 mol/L of NaOH. For the next
5 minutes, the concentration of unreacted NaOH is 0.022 mol/L. The concentration of
NaOH decreases as time increases. After 25minutes, the concentration of NaOH is
decreasing to 0.0146 mol/L. Thus, it is proved that as residence time increases, the
concentration of the reactant exiting the reactor decreases.
In addition, as shown in figure 6, graph of time versus 1/CA is plotted which increasing in
a straight line. Thus, it is proved the order for the reaction at 29.9oC is 2nd order. The rate
constant, k for the reaction at 29.9oC is 1.3775 L/mol.min which is taken from the slope of
second order graph.
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9.2 Effect of Temperature
In this Continuous Stirred Tank Reactor (CSTR) experiment, the reaction occurs between
NaOH and Et(Ac) in a CSTR model BP-100. The concentration of unreacted NAOH can
be calculated based on volume of NaOH titrated. Thus, the order of the reaction of each
temperature can be identified based on the rate of concentration of the reactant by plotting
a graph. Firstly, before plotting the graph, the number order of the reaction on the each
temperature is identified by guessing the number of order either zeroth, first, second or
third order. Then the graph of time versus CA, log CA, 1/ CA or 1/ CA 2 which also represented
zeroth order, first order, second order or third order respectively is plotted. The equation
for the rate law which is –rA can be determine using the equation of slope based on graph
–rA=mx + c.
This CSTR experiment used two different method in order to calculate rate constant, k to
varying the temperature. Based on graph plotted in figure 16 where the linear line equation
is y = 9040x + 28.973 is obtained from the slope. Graph of ln k vs 1/T shows increasing
trend. By using the linear line equation, Ea is calculated which is -75158.56J/mol. While
using the other method which is Arrhenius equation, the activation energy obtained is -
76004.05 J/mol. From these two value from two different method, the deviation obtained
is very small value which is 1.11%.
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10.0 CONCLUSION
The Continuous Stirred Tank Reactor (CSTR) experiment which is the saponification of NaOH
and Et(Ac) is conducted by observed the saponification process where for every 5minutes the
sample from each temperature is collected. The sample mixture is then titrated in order to
obtain the concentration of unreacted NaOH. In conclusion, by plotted graph from
concentration obtained, the saponification process occurs at 2nd order based on the graph
1/CA of the reaction at 29.9oC, 40oC and 50oC. At 29.9oC the concentration of NaOH decreases
as residence time increases. At first minute, the concentration of NaOH is 0.029 mol/L, while
after 25 minutes, the concentration of NaOH is 0.0146mol/L. Hence, it is proved that
concentration of reactant depends on the reaction time which also developed a high rate of
reaction in a chemical processes. Other than that, the rate constant, k is also increases as the
temperature of reaction increases. From this experiment, the –rA obtained for 40oC is 0.00022
mol/min.L, while at 50oC the –rA is 0.00054 mol/min.L. From this result, it shows that the rate
of reaction also depends on the temperature of a reaction. As the temperature of reaction
increases, the rate of reaction also increase. Lastly, from this experiment, it is shows that the
activation energy of a reaction is same at a same concentration but varying reaction of
temperature. Two method are used in order to calculate the activation energy by using the
equation of slope and the Arrhenius of equation. From two value obtained, it has only small
deviation. Thus, it is proved that both equation is valid. The CSTR experiment is success and
all the objectives are achieved.
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11.0 RECOMMENDATION
A few recommendations are suggested on the techniques employed during the experiment
which is before doing the experiment, students should do some research on how the
experiment should be done. This is to ensure the students are able to conduct the experiment
well besides to avoid any error throughout the experiment. As a preparation, table of data
should be done before the experiment start in order to ensure the data is recorded correctly.
During the experiment, students should adjust the flow rate of the reactor at the exact set
value in litre per minute. This is because the value of the flow rate is not fix over time, it is
automatically kept changing the desired value. Thus, students should manually adjust the flow
rate value into the desired value.
Besides, the other recommendation should employed is during the titration, the colour
changes should be consistent at light pink. Titration should be done accurately. Eyes should
be perpendicular when taking the reading of pipette.
Last but not least, the drain valve should be drain completely before continue with other
temperature. Furthermore, when taking the sample, the valve should be drain a few seconds
before collect the sample in order to remove the previous mixture of reaction.
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12.0 REFERENCES
J.T. Ugye, A. U. (2013). Temperature Effects on the Rate of Reaction of Plasma Albumin with
Formaldehyde in Water Solution and Ethanol-Water-Mixtures. Chemistry Journal, 128-132.
Ward, C. A. (August, 1983). Effect of concentration on the rate of chemical reactions. The Journal of
Chemical Physics, 79(11).
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APPENDIX
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