ABSTRACT

At first, we mix Ethyl Acetate (1.25L) and sodium hydroxide (NaOH) (1.25L) with
equal volume in the reactor. Then we set the temperature at 30 oC and start the experiment by
turn on the stirrer. For the first sample, we take after 1 min. After that, every 5 min. Sample
that has been take we mix it with Hydrochloric acid (HCL) and 3 drops of Phenolphthalein.
Then we titrate with 0.1M NaOH. The volume of NaOH used was been record in the result.

We proceed the experiment with temperature 40 oC. When all the result has been
taken, calculation was made and we plot a graph based on that result. By the graph we can
determine the rate of the reaction.

INTRODUCTION

The chemical reactors are something that is crucial and important in a chemical
industries. It is the most important things as it is the place for the reaction to happen. The type
of reactor must be suited with the reaction that we seek for. One of the example of the reactors
is Continuous Stirred Tank Reactor (CSTR).

CSTR are open systems, where material is free to enter or exit the system, that operate
on a steady-state basis, where the conditions in the reactor don't change with time. Reactants
are continuously introduced into the reactor, while products are continuously removed.

CSTR are very well mixed, so the contents have relatively uniform properties such as
temperature, density, etc. throughout. Also, conditions in the reactor's exit stream are the same
as those inside the tank.

The CSTR is equip with a stirring blade or agitator, water jacket, heat exchanger and
also the water inlet and outlet. The CSTR usually used for a homogenous reaction in a
industrial processing where constant mixing is required.

1
OBJECTIVE

To study the effect of temperature on reaction rate constant, k for batch reaction and study the
activation energy of saponification.

THEORY

Consider the chemical reaction as below:

aA + bB cC + dD

Residence time, is the average amount of time that a particle spends in a particular
system. The residence time, is a representation of how long it takes for the concentration to
significantly change in the sediment.

Where VCSTR is the reactor volume and vo is the total feed flow rates. The reactor
volume and the total feed flow rates for each experiment remain unchanged.

Conversion and its related terms yield and selectivity are important terms in chemical
reaction engineering. They are described as ratios of how much of a reactant has reacted, how
much of a desired product was formed and how much desired product was formed in ratio to
the undesired product(s). Conversion XA is the number of moles of A that have reacted per
mole of A fed to the system.

A reaction rate constant, k quantifies the rate of a chemical reaction. The reaction rate
is often found to have the form.

2
 Where CA and CB are the concentration of the species A and B respectively, each
raised to the powers and , while k is the reaction rate constant. The exponents and
are the partial reaction orders.

Since the experiment that we had carried out is temperature dependence, we use the
Arrhenius equation. The Arrhenius equation gives the quantitative basis of the relationship
between the activation energy and the reaction rate at which a reaction proceeds. The rate
constant is then given by

() =

From the Arrhenius equation above, we can derive a new formula to find activation
energy, E.

1
ln = ln ( )

= (ln ln )

Where, E is the activation energy ,A is the Arrhenius constant, R is the Universal Gas
Constant which is 8.314 J/mol.K , and T is the absolute temperature. Activation energy, E is
the minimum quantity of energy that the reacting species must possess in order to undergo a
specified reaction.

3
MATERIAL AND APPARATUS

Material :

1. Ethyl Acetate - Et(Ac)

2. Sodium Hydroxide - NaOH
3. Hydrochloric Acid - HCL
4. Phenolphthalein

Apparatus :

Control Panel

Reactor

Figure 1 : CSTR

4
PROCEDURE

1. The overflow tube in the reactor is being adjusted to give a desired working volume
(2.5liters). The pump P1 was switched on to start on pumping 1.25 liters of 0.1M ethyl
acetate form the feed tank into reactor. The pump P1 stopped.

2. Then the pump P2 was switch on and starts to pump another 1.25 liters of the0.1M
NaOH into the reactor. When the 2.5 liters volume is reached, then the pump P2 were
being stopped. The temperature was set at 30C. The stirrer then being switches on
and the speed was set in the mid- range (180rpm). The time is being observed. The
start time are recorded.

3. 10ml of the 0.25M HCL were quickly measured in a flask.

4. After 1 minute of reaction, sampling valve V7 opened to collect 50ml sample.10ml of

the 0.25M HCL are immediately added into the sample. The HCL quench the reaction
between ethyl acetate and sodium hydroxide.

5. The mixture was titrated with the 0.1M NaOH to evaluate the amount of un-reacted
HCL. This had provided us with the information to determine the amount NaOH in
feed solution which has reacted.

6. Steps 4 and 5 were repeated for reaction times of 5, 10, 15, 20 and 25.

7. The experiment was repeated for reaction temperatures 40 C.

8. The graph 1/CA vs. t and ln k vs. 1/T were plotted.

9. The activation energy was found from the ln k vs. 1/T graph.

5
RESULT AND CALCULATION

1) For temperature 30 oC

Volume of
Time (min) NaOH used CA (mol/L) 1/CA (L/mol)
for titration
(mL)
1 2 Average
1 9.10 9.50 9.30 0.0320 31.25
5 6.60 5.80 6.20 0.0376 26.60
10 7.30 9.20 8.25 0.0335 29.85
15 6.20 6.90 6.55 0.0369 27.10
20 8.00 7.30 7.65 0.0347 28.82
25 7.8 13.20 10.50 0.0290 34.48

2) For temperature 40 oC

Volume of
Time (min) NaOH used CA (mol/L) 1/CA (L/mol)
for titration
(mL)
1 2 Average
1 6.30 6.40 6.35 0.0373 26.81
5 7.90 8.50 8.20 0.0336 29.76
10 8.70 8.60 8.65 0.0327 30.58
15 8.40 8.90 8.65 0.0327 30.58
20 8.80 9.00 8.90 0.0322 31.06
25 8.90 8.50 8.70 0.0326 30.67

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Temperature : 30 oC

Graph 1/Ca vs t
40
35
30 y = 0.1251x + 28.098
1/CA (L/MOL)

25
20
15
10
5
0
0 5 10 15 20 25 30
TIME (MIN)

k = 0.1251 L/mol.min

Temperature : 40 oC

GRAPH 1/Ca VS t
32
y = 0.1328x + 28.228
31

30
1/CA (L/MOL)

29

28

27

26
0 5 10 15 20 25 30
TIME (MIN)

k = 0.1328 L/mol.min

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 ln k vs 1/T
-2.01
0.00318 0.0032 0.00322 0.00324 0.00326 0.00328 0.0033 0.00332
-2.02

-2.03
LN K (L/MOL.MIN)

-2.04

-2.05

-2.06

-2.07
y = -563.21x - 0.2206
-2.08 R = 1
-2.09
1/T

Slope = -562.21

Sample of Calculations

At 30 oC :

Volume of unreacted quenching HCL, V1 :

V1 = (CNaOH / CHCL) volume of titrated NaOH

= (0.1 mol.L-1 / 0.25 mol.L-1 ) 9.3 mL

= 3.72 mL

Volume of HCL reacted, V2 :

V2 = VHCL V1

= 10 mL 3.72 mL

= 6.28 mL

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Moles of reacted HCL, n1 :

n1 = CHCL V2

= 0.25 mol/L 6.28 mL 1 L/1000mL

= 0.00157 mol

Moles of unreacted NaOH in sample, n2 :

n2 = n1

= 0.00157 mol

Concentration of unreacted NaOH, CNaOH :

CNaOH unreacted = n2 / volume sample

= 0.00157 mol / 0.05 L

= 0.0314 mol/L

1/CA = 1 / 0.0320 mol/L

= 31.25 L/mol

Reaction rate constant, k :

= From the slope of the graph

9
To calculate the rate of reaction, -rA :

-rA = kCA 2

= (0.1251 L/mol.min)(0.0314 mol/L)2

= 1.2334 10-4 mol/L.min

To calculate the activation energy from the reaction :

From the graph ln k vs 1/T, the equation for the best fit is

y = -563.21x - 0.2206

ln k = -563.21(1/T) - 0.2206

Activation energy from Arrhenius equation

2 1 1
ln = ( )
1 1 2

0.1328 1 1
ln = ( )
0.1251 8.314 303.15 313.15

Ea = 4714.31 J/mol

From slope graph ln k vs 1/T :

Slope = -Ea/R

-563.21 = -Ea/8.314

Ea = 4682.53 J/mol

10
DISCUSSION

This experiment is to study the effect of temperature on reaction rate constant, k for
batch reaction and determine the activation energy of saponification. Batch Stirred Tank
Reactor is one of the reactors that widely used in industrial. Batch stirred Tank reactor is a
closed system. For this experiment we used liquid that have a constant density. For that it is a
constant-volume Batch reactor.

In this experiment, the ethyl acetate and sodium hydroxide were mixed in the reactor
at 30 oC. As the stirrer was switched on, the solution began to mix. After 1 minutes, the
sample was collected from sampling tube. Our group take 2 sample to get the average reading.
The solution were quickly mixed with 10 mL of 0.25M HCl and 3 drops of phenolphthalein.
Then, this solution was titrated with 0.1M of NaOH. The titration stop when the color of
solution changes from clear to light pink. The value of NaOH used to titrate the solution were
recorded. The average value recorded was 9.30 mL. The experiment continue by taking the
sample after 5 minutes, 10 minutes, 15 minutes, 20 minutes and 25 minutes. The average
value recorded are 6.20 mL, 8.25 mL, 6.55 mL, 7.65 mL and 10.50 mL respectively.

The experiment was repeated at temperature 40 oC. The cooling water needed as to
control to maintain the temperature of reactor. The solution first mixed and heated to 40.
Then stirrer was switched on and the time is start.

After 1 minutes, the sample of solution was collected and been mixed with 10 mL of
0.25M HCl and 3 drops of phenolphthalein. Then, this solution was titrated by 0.1M of NaOH
until the color changes to light pink. The value were recorded. The average value are 6.35
mL. The experiment continue by taking the sample after 5 minutes, 10 minutes, 15 minutes,
20 minutes and 25 minutes. The average value recorded were 8.20 mL, 8.65 mL, 8.65 mL,
8.90 mL and 8.70 mL respectively.

11
 The value of concentration of unreacted ethyl acetate was calculated by using some
formula. The details in RESULT AND CALCULATION. The graph 1/Ca vs time was plotted
for the 2 temperature. From the slope of graph, the value of k can be determine. The value of
k are 0.1251 for 30 and 0.1328 for 40 . From this k value, the graph of ln k vs 1/T have
been plotted. The activation energy can be calculated from this graph. Slope of the graph is
equal to Ea/R. The value of Ea calculated was 4682.53 J/mol. As the value is positive its
shown that this reaction is endothermic reaction.

CONCLUSION

In this experiment I can conclude a few thing. 1st conclusions were that this equation
is elementary and it is 2nd order. I conclude this by the graph 1/Ca versus t (time) that has
been plotted. I get straight line graph that has a positive slope value. My second conclusions
that the value of k is dependent on temperature and the rate constant will only constant for a
constant temperature. When the temperatures increase the value of reaction rate also increase.
This satisfied the Arrhenius equation

() =

I also conclude that activation energy is constant for reactions that have same concentration
but different temperatures. This has been proven by the equation
2 1 1
ln = ( )
1 1 2

and the graph that I have plotted. I get almost the same value.

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RECOMMENDATIONS

i. The temperature should be optimize at the set point accurately as the temperature
could affect the reaction.
ii. Make sure to purge out the solution used in previous experiment before start the new
experiment to ensure that the reaction is freshly mixed to get more accurate value.
iii. Make sure do titration gently as the value could be affected by doing it fast.
iv. Take 3 reading to get average results and more accurate.
v. Make sure to recheck the equipment before start the experiment to make sure all
switch is on.

REFERENCES

1) Saponification Theory by Helena Shomar, retrieved from

http://www.livingashes.net/saponification-theory/
2) Saponification Definition and Reaction by Anne Marie, retrieved from
https://www.thoughtco.com/definition-of-saponification-605959
3) Sakshat Virtual Labs, Continuous stirred reactor, retrieved from
http://iitkgp.vlab.co.in/?sub=35&brch=107&sim=1175&cnt=1
4) College of Engineering, University of Michigan. Continuous Stirred Tank Reactors,
retrieved from
http://encyclopedia.che.engin.umich.edu/Pages/Reactors/CSTR/CSTR.html
5) Wikipedia. Continuous Stirred-Tank Reactors, retrieved from
https://en.wikipedia.org/wiki/Continuous_stirred-tank_reactor

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APPENDIX

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