1.

0 ABSTRACT
This experiment is conducted in order to achieved a few aims or objectives. The experiment
is to carry out a saponification reaction between NaOH and Et(Ac) in continuous stirred tank
reactor or commonly known as CSTR. The objectives for this experiment are to determine the
effect of residence time onto the reaction extent of conversion and to determine the reaction
of rate constant and lastly to determine the reactions activation energy. In order to conduct
this experiment a continuous stirred tank reactor model BP 143 is used. Before we started, we
ensured that all the general start up was carried out properly to avoid any mistake that will
effect the result obtained. The experiment is started by opening valves V5 and V10 to obtain
the highest possible flow rates that can be achieve. Then, the readjust valves V5 and V10 to
achieve 0.1 L/min but both flow rates reading must be the same for valves V5 and V10. This
steps is repeated by different value of flow rates which is 0.15, 0.20, 0.25, and 0.30 L/min.
For each flow rate s50 mL of sample will be collected in order to carried to a back titration.
The stable conductivity is recorded into a data for every 5min before collect the samples. In
the back titration, the samples that had been collected are titrated with NaOH for
saponification reaction until it change colour from colourless into light pink. Then, the
amount of NaOH titrated were recorded. From the tabulated data, a few of calculation are
carried out and graph had been plotted.

2.0 INTRODUCTION
One of the important component in the industrial sector that help the operation of the factory
to produce products is a reactor. A reactor will change a raw product into the desire product
that are needed. The right criteria for a good reactor is it can produce a high production with a
great quality and economical. A common type of reactor that usually used in the industry is
the mixing or stirred reactor. One of the stirred reactors is Continuous Stirred Tank Reactors
(CSTR) this reactor is a common ideal reactor type in chemical engineering. Majority in
chemical process industry, CSTR is being used as an equipment which is raw materials
undergo a chemical change in order to form desired product. The types of process for this
equipment is steady state because most of the this reactor will operate at steady state and it is
assume to be in perfectly mixed. The CSTR reactor used are commonly used in industrial
processing, primarily in homogeneous liquid-phase flow reactions, where constant agitation
is required.

Figure 1 Cross-sectional diagram of Continuous stirred-tank reactor

As for this experiment a continuous stirred tank reactor ,CSTR (model : BP 143) is being
used.
The CSTR can run as single reactor and also in series. The CSTR that connected in series,
the exit stream of one reactor is the feed stream for another reactor. There are three reactor
vessels connected in series by piping, each containing a propeller agitator driven by a
variable speed electric motor and the unit based on the simplest classic case of well mixed,
multi-staged process operation. The solution in each reactor is well stirred and the
concentration can be measured. These three reactors are to compare the measured responses
of the vessel concentrations to deliberate change at the inlet with a theoretical prediction.

Figure 2 Single Continuous Stirred Tank Reactors (CSTR)

Figure 3 Continuously Stirrer Tank Reactor (CSTR) in series.

3.0 OBJECTIVE
The objective of this experiment are :
To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
To determine the effect of residence time onto the reaction extent of conversion
To determine the reaction rate constant
To determine the reactions activation energy
4.0 THEORY
Saponification is a process where alkaline hydrolysis the fatty acid ester. In this experiment it
is involved hydrolyzed of esters in fat by sodium or potassium hydroxide (NaOH or KOH) to
produce a carboxylate anion which can act as surfactant for example soap. The equation
below shows the saponification process between sodium hydroxide and ethyl to produce
sodium acetate and by product ethanol.
C2H5O2CCH3
Ethyl Acetate

+ NaOH

CH3CO2Na +
H3CCH2OH
Sodium Hydroxide Sodium Acetate
Ethanol

As for the experiment preparation of calibration curve for conversion vs conductivity, the
reaction that need to be studied in this experiment is the saponification reaction of ethyl
acetate Et(Ac) and sodium hydroxide (NaOH). Since this is a second order reaction, the rate
of reaction depends on both concentrations of Et(Ac) and NaOH. However, for analysis
purposes, the reaction will be carried out using equimolar feeds of Et (Ac) and NaOH
solutions with the same initial concentrations. This ensures that both concentrations are
similar throughout the reaction.
NaOH + Et (Ac)

Na(Ac) + EtOH

From this experiment, it is required to calibrate the conductivity measurements of conversion

values for the reaction between 0.1 M ethyl acetate and 0.1 M sodium hydroxide. The
conversion will start from 0% conversion, 25% conversion, 50% conversion, 75%
conversion, and 100% conversion. Each of the conversion contains different amount NaOH,
Et(Ac), and deionised water for example for 0% conversion there will be 100 mL of NaOH,
for 75% conversion will contains 25 mL of NaOH + 75 mL Et(Ac), and for 100% conversion
it will contain 100 mL of Et(Ac). Different percentage of conversion will give different value
of conductivity.
For back titration procedure it is advisable to carry out manual conversion determination on
experiment samples to verify the conductivity measurement values. It is based on the
principle of quenching the sample with excess acid to stop any further reactions, then back
titrating with a base to determine the amount of unreacted acid.
NaOH + HCl
The back titration can be calculate as follow :
Conc. of NaOH entering the reactor, (CNaOH,o)
C NaOH , f
2
Volume of unreacted quenching HCl, (V2)
C NaOH , s
V 1
C HCl, s

NaCl + H2O

Vol. of HCl reacted with NaOH in sample, (V3)

V HCl , sV 2
Moles of HCl reacted with NaOH in sample, (n1)
C NaOH , s

V3
1000

Moles of unreacted NaOH in sample, (n2)

n2=n1
Conc. of unreacted NaOH in the reactor, (CNaOH)
n2
Vs
1000
Conversion of NaOH in the reactor, X
NaOH
100
(1 CCNaOH
,o )
Reaction rate constant
K = (CAO- CA)
CA2
5.0 APPARATUS
1.
2.
3.
4.
5.

Continuous stirred tank reactor (Model : BP 143)

50 mL burette
200 mL beaker
Conical flask
Solution :
i.
Sodium hydroxide, NaOH (0.1M)
ii.
Sodium acetate, Et(Ac) (0.1 M)
iii.
Deionised water, H2O
iv. Hydrochloric acid, HCL (0.25M)
v. Phenolphthalein
6. Conductivity probe
7. 100 mL measuring cylinder.

Figure
6.0 PROCEDURE
GENERAL START-UP PROCEDURE :
1. The following solutions are prepared :
I.
40 L of sodium hydroxide, NaOH (0.1M)
II.
40 L of ethyl acetate, Et(Ac) (0.1M)
III.
1 L hydrochloric acid, HCL (0.25M), for quenching
2. All valves are ensured initially closed.
3. The feed vessels are charged as follows:
I.
The charge port caps for vessels B1 and B2 ae opened
II.
NaOH solution is poured carefully into vessels
4. The power for the control panel is turned on.
5. The water in the thermostat T1 tank is checked. Refilled as necessary.
6. Cooling water valve V13 is opened and the cooling water is let to flow through the
condenser W1. (only for experiment 2)
7. The overflow tube is adjusted to give a working volume of 10 L in the reactor R1.
8. Valves V2, V3, V7, V8, and V11 are opened.
9. The unit is now ready for experiment.

PREPARATION

OF CALIBRATION

CURVE

FOR

CONCENTRATION

VS

CONDUCTIVITY
1. The following solutions are prepared :
I.
1 liter osf sodium hydroxide, NaOH (0.1M)
II.
1 liter of sodium acetate, Et(Ac) (0.1)
III.
1 liter of deionised water, H2O
2. The conductivity and NaOH concentrationfor each conversion values by mixing the
following solutions into 100 mL of deionised water are determined :
I.
0% conversion
: 100 mL NaOH
II.
25% conversion : 75 mL NaOH + 25 mL Et(Ac)
III.
50% conversion : 50 mL NaOH + 50 mL Et(Ac)
IV. 75% conversion : 25 mL NaOH + 75 mL Et(Ac)
V. 100% conversion : 100 ml Et(Ac)

BACK

TITRATION

PROCEDURES

FOR

MANUAL

CONVERSION

DETERMINATION
1. Aburette is filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl in a flask.
3. 50 mL sample is obtained from the experiment and the sample is immediately added
to the HCl in the flask to quench the saponification reaction.
4. A few drops of pH indicator are added into the mixture.
5. The mixture is titrated with NaOH solution from the burette until the mixture is
neutralized. The amount of NaOH titrated is recorded.

EXPERIMENT 1 : EFFECT OF RESIDENCE TIME OF THE REACTION IN A

CSTR.
1. The general start-up procedure is performed.
2. Both pumps P1 and P2 are switched on simultaneously and valves V5 and V10 are
opened to obtain the highest possible flow rate into the reactor.
3. The reactor is let to fill up with both the solution until it is just about to overflow.
4. The valves V5 and V10 are readjusted to give a flow rate of about 0.1 L/min. Both
flow rate are make sure to be the same. The flow rate is recorded.
5. The stirrer M1 is switched on and the speed is set to about 200 rpm.
6. The conductivity value at Q1-401 ia started monitoring until it does not change over
time.The reactor is ensured had reached steady state.

7. The steady state conductivity value is recorded and the concentration of NaOH in the
reactor is found and extent of conversion from the calibration curve.
8. Sampling valve V12 is opened and 50 mL sample is collected. A back titration
procedure is carried out to manually determine the concentration on NaOH in the
reactor and extent of conversion.
9. The experiment are repeated from steps 5 to 9 for different residence times by
adjusting the feed flow rates of NaOH and Et(Ac) to about 0.15, 0.20, 0.25 and 0.30
L/min. Both
flow rates are make sure the same.

EXPERIMENT 2 : EFFECT OF TEMPERATURE ON THE REACTION IN A CSTR

1. The general start-up procedures are performed.
2. Both pumps P1 and P2 are switched on simultaneously and valves V5 and V10 are
opened to obtain the highest possible flow rate into the reactor.
3. The reactor is let to fill up with both the solution until it is just about to overflow.
4. The valves V5 and V10 is readjusted to give a flow rate of 0.20 L/min. Both flow
rates is make sure the same. The flow rates are recorded.
5. The stirrer M1 is switched on and the speed at about 200 rpm is set.
6. The thermostat T1 is switched on and the water temperature is set to 40 oC.
7. The conductivity value at Q1-401 are started monitoring and the temperature value at
T1-101 until they do not change over time.This is to ensure that the reactor has
reached steady state.
8. The steady state conductivity value and temperature values are recorded and the
concentration of NaOH in the reactor is found and extent of conversion from the
calibration curve.
9. Sampling valves V12 is opened and 50 mL sample is collected. A back titration
procedure is carried out to manually determine the concentration of NaOH in the
reactor and extent of conversion.
10. The experiment is repeated from steps 7 to 10 for different reactor temperatures by
setting the thermostat temperature to 50, 60, 70, and 80 oC. The flow rates of both
solutions are mainteained at 0.20 L/min.
GENERAL SHUT-DOWN PROCEDURE
1. The cooling water valve V13 is kept open to allow the cooling water to continue
flowing.
2. Both pumps P1 and P2 are switched off. Stirrer M1 is switched off.

3. The thermostat T1 is switched off. The liquid in the reaction vessel R1 is let to cool
down to room temperature.
4. Cooling water valve V13 is closed.
5. Valves V2, V3, V7 and V8 are closed. Valves V4, V9 and V12 are opened to drain any
liquid from the unit.
6. The power for the control panel is turned off.
7.0 RESULTS
Conversion

Solution mixtures
0.1 M NaOH 0.1
M H2O

Concentratio

n of NaOH (mS/cm)

Et(Ac)
0%
25%
50%
75%
100%

Bil.

1.
2.
3.
4.
5.

100 mL
75 mL
50 mL
25 mL
-

25 mL
50 mL
75 mL
100 mL

Flow

(oC)

NaOH, (L/min)
29.8
30.0
30.2
30.4
30.5

(M)
0.0500
0.0375
0.0250
0.0125
0.0000

100 mL
100 mL
100 mL
100 mL
100 mL
Table 1

Temperature

rate

Conductivity

14.490
8.990
4.750
3.150
0.127

of Flow rate of Et(Ac), Total flow rate of Residence

(L/min)

0.10
0.15
0.20
0.25
0.30

solution,Fo,(L/min)
0.10
0.15
0.20
0.25
0.30

0.20
0.30
0.40
0.50
0.60

time,

(min)
200.00
133.33
100.00
80.00
66.67

Table 2

Property
Formula
Appearance
Molecular weight
Normal boiling point
Normal melting point
Density
Refractive index

Ethyl acetate
CH3COOCH2CH3
Clear liquid
88.11 g/mol
77.1 oC
-84.0 oC
0.8945 g/mol @ 25 oC
1.3274 @ 20 oC

Sodium hydroxi
NaOH
White solid
40.00 g/mol
1390 oC
323 oC
2.1 g/mol
-

Table 3

8.0 CALCULATIONS
Conc. of NaOH entering the reactor, (CNaOH,o)

C NaOH , f
2
0.1 M
2

= 0.05 M
Volume of unreacted quenching HCl, (V2)

C NaOH , s
V 1
C HCl, s
0.1 M
x 21.8 mL
0.25 M

= 8.72 mL
Vol. of HCl reacted with NaOH in sample, (V3)

V HCl , sV 2
= 10 mL 8.72 mL
= 1.28 mL
Moles of HCl reacted with NaOH in sample, (n1)

C NaOH , s

V3
1000

0.25 M x 1.28 mL
1000
= 3.2 x 10-4

Moles of unreacted NaOH in sample, (n2)

n2=n1 = 3.2 x 10-4

Conc. of unreacted NaOH in the reactor, (CNaOH)

n2
Vs
1000
=

3.2 x 104
1000
50

mol
L

= 6.4 x 10 -3

Conversion of NaOH in the reactor, X

NaOH
100
(1 CCNaOH
,o )
6.4 x 103
) x 100
0.05

= (1

= 87.2
A. Reaction rate constant
K = (C AO- CA)
C A2
= 0.05 (6.4 x 10-3)
200 (6.4 x 10-3)2

= 5.3223
-rA = kCA2
= 2.1800 x 10-4

m
s

Conductivity vs Conversion
16
14
f(x) = - 3.46x + 16.67

12
10

Conductivity (mS/cm)

8
6
4
2
0

25

50

Conversion, X (%)

75

100

Graph 1

conversion vs residence time

87.5
87
f(x) = 0.01x + 84.92
86.5
86

Conversion,X (%)

85.5
85
84.5
84
60

80

100

120

140

160

180

200

220

Residence time (min)

Graph 2

9.0 DISCUSSION
The Experiment is conducted to determine the reaction rate constant and also to determine the
effect of residence time on the conversion in a continuous stirred tank reactor (CSTR).
Continuous stirred tank reactor (Model : BP 143) is used in this experiment to predict the
behaviour of chemical reactor thus, the dimension of the reactor can be estimated.
The experiment is conducted with setting up the flow rate of both NaOH and Et(Ac) into 0.10
L/min, and the experiment are repeated by using different value of flowrate which are 0.15

L/min, 0.20 L/min, 0.25 L/min and 0.30 L/min. From the experiment conducted, the data
shown that when the flow rates of the reactant in the reactor become higher, the residence
time tends to decrease. Residence time is known as the removal time which is the average
amount of time that a particle spends in a particular system. It can be said that the relationship
between the flow rates and the residence time is inversely proportional.
From the data obtained from the experiment, graph conductivity versus residence of time is
plotted. From the graph we can see that the value that we get from the experiment have some
error. Graph that we supposed to get is conversion is directly proportional to the residence
time which is the value of conversion will be increase as the time increase \but the result that
we obtained from the experiment are at 0.10 L/min the value of conversion is 87.2%, at 0.15
L/min the value of conversion is dropped to 85.2% but at 0.20 L/min the value of conversion
is raised back to 86.0%, at 0.25 L/min the value of conversion continued to raised to 87.2%
and after that the value of conversion dropped back to 85.2% for flow rate 0.30 L/min. From
the observation the value obtained does not fit the theoretical theory for this experiment. So
we assume that during conducting the experiment some error must have occur.

10.0 CONCLUSION
For this experiment, continuous stirred tank reactor (CSTR) is used. The objective for this
experiment is to determine the reaction rate constant and also the effect of residence time on
the conversion. From the results that we obtained we know that some errors does occur
during the experiment that effect the result. The theoretical result that shows that the graph
for conversion vs residence time must be directly proportional but the result that obtained
from the experiment show some fluctuated in the graph. So we considered as the experiment
does not achieved its objectives.

11.0 RECOMMENDATION
1. Make sure reactor does not have any leaks and valve closed and opened as needed,
controlled the valve carefully and slowly when adjusting the flow rate to obtain 0.10
L/min. Make sure that the flow rate stable then start the experiment.
2. To get a better result, only one person is needed to take care of the opening and
closing of the valve and other person take care of the pump. This is because some
valve needed to be opened or closed simultaneously.
3. Make sure the tank is filled with the correct solution and to the correct amount.
Different substance reacts differently and lack of substance can damage the apparatus.
4. Make sure general start-up procedure is done first in order to check the machine
functionality.
5. Sodium hydroxide is corrosive to flesh and it can cause blindness. To prevent this
from happen, eye protection should be wear at all the time and make sure to wear
gloves when dealing with it.
6. All of the apparatus should be rinse properly to avoid any reaction happen before
testing it. Wash and dry it properly in order to get accurate result especially for
titration.
7. Repeat the titrationsnfor two or three times because a lot of error comes from titration.

12.0 REFERENCE
1. Levenspiel, O., Chemical Reaction Engineering, 3rd ed.,John Wiley and Sons, New York, 1999.

2. Retrieved 11th April 2016 , from

https://en.wikipedia.org/wiki/Sodium_hydroxide#Saponification
3. Retrieved 11th April 2016 , from
https://en.wikipedia.org/wiki/Continuous_stirred-tank_reactor
4. Retrieved 11th April 2016 , from
http://www.umich.edu/~elements/5e/asyLearn/bits/cstr/index.htm
5. Retrieved 11th April 2016 , from
http://encyclopedia.che.engin.umich.edu/Pages/Reactors/CSTR/CSTR.html

13.0 APPENDIX