Faculty of

Chemical
Engineering
REPORT

POLLUTION CONTROL & CHEMICAL REACTION ENGINEERING

LABORATORY
(SKTK3731)
2020/2021-SEM 1

EXPERIMENT
Experiment 2:
Saponification of Ethyl Acetate and Sodium Hydroxide in CSTR

LAB INSTRUCTOR
Assoc. Prof. Dr. Mukhlis bin A. Rahman

SECTION 03
GROUP 04

NO. TEAM MEMBERS MATRIC NO.

MUHAMMAD SHAFIQ HAQIMI BIN
1. A18KT0188
MOHD ESLI
MUHAMMAD ZAKWAN BIN
2. A18KT0191
NAJOHAN
NAEIMATUL HIDAYAH BINTI
3. A18KT0197
ABDUL GHANI
NOR AINA SAHIRA BINTI MOHD
4. A18KT0206
SAIFUDDIN
 Table of Contents
1.0 ABSTRACT..................................................................................2

2.0 INTRODUCTION........................................................................3

3.0 LITERATURE REVIEW.............................................................5

4.0 THEORY......................................................................................5

5.0 METHODOLOGY.......................................................................7

6.0 RESULT.......................................................................................8

7.0 DISCUSSION.............................................................................20

8.0 CONCLUSION...........................................................................23

9.0 REFERENCES...........................................................................23

10.0 APPENDICES............................................................................23

1
 1.0 ABSTRACT

The purpose of the experiment is to study the saponification reaction of sodium hydroxide
an ethyl acetate in a Continuous–Stirred Tank Reactor (CSTR). Besides, this experiment was
carried out to investigate the operational behaviour in CSTR and learn to operate the CSTR
system. The final objective was to verify the reaction order and the rate constant of
saponification reaction between sodium hydroxide and ethyl acetate by using graphical
technique (concentration vs time data) and analytical technique which is from design equation
of CSTR and the results from both technique will be compared. Finally, the reaction kinetics,
rate law and conversion in batch reactor to the one in a CSTR system for the same reaction
will also be compared.

First of all, before all apparatus is set-up, the conductivity calibration curve with
different molar concentration was prepared to determine reaction kinetics and rate law of the
process. Then, the experiment was carried out according to the procedure and data obtained is
recorded on the results table. The process was repeated several times using different feed of
flow rates. The calculation of the concentration of input and output chemicals, rate of reaction
and theoretical space time of CSTR are based on the theory. Instead of that, the discussion
section shows the graph plotted using the result obtained and discussed it more detail based on
chemical reaction theory.

From the result obtained, it shows that on the graph concentration versus time, we get
the value of rate constant by using graphical method, k = 0.9051 L/mol.min and little bit
differ by using analytical method which is k = 0.6435 L/mol.min. Other than that, the reaction
order is successfully to approve that it is second order of reaction based on linear graph of
concentration versus time. The errors and recommendations also were discussed in the
discussion section. The conclusion section concludes all the objectives and calculations on
this experiment.

2
 2.0 INTRODUCTION

The Continuous-Stirred Tank Reactor (CSTR) is common type for chemical reactor in
chemical engineering and environmental engineering. It is commonly used in industrial
processing which is primarily used for liquid phase reaction. In these reactors, reactants are
continuously flowed into the reactor, where they undergo chemical reaction. Simultaneously,
an exit stream is extracted from the reactor at the same flow rate as inlet stream to maintain
constant volume inside the reactor. Because the contents of the reactors are constantly stirred,
the feed and product is assumes in a uniform composition throughout the reactor. The
advantage of CSTR is it allows for the continuous production of the desired product without
the need to repeatedly empty and fill the tank. Besides that, it has good temperature control,
easily adapt to two phases, low operating cost and easy to clean. Unfortunately, the CSTR has
lowest conversion per unit volume and requires large volume to obtain the desired
conversions. Operating large reactors in industry can be expensive, so a common trick used to
reduce a cost is to operate multiple CSTRs in series. Equally good results can be obtained by
dividing a single vessel into compartments while minimizing back-mixing and short-
circuiting. The larger the number of CSTR stages, the closer the performance approaches that
of a tubular plug-flow reactor.

This experiment was carried out to study the saponification reaction between sodium
hydroxide and ethyl acetate in a continuous – stirred tank reactor (CSTR). This process was
conducted to produce soap, usually from fat and lye. Technically, the saponification process
involves base (caustic soda NaOH) hydrolysis of triglycerides, which are ester of fatty acids,
to form sodium salt of carboxylate.

Instead of carrying out saponification reaction, the other scopes of this experiment are to
investigate the operational behavior of a reaction in CSTR, to calculate the reactant
conversion based on the conductivity calibration curve. Also, the significance of doing this
experiment was to verify the reaction order obtained from the hypothesis of the experiment
and to determine the rate constant of saponification reaction between sodium hydroxide and
ethyl acetate using graphical and analytical technique.

3
 Then, the results from both techniques were compared. In fact, the experiment was
conducted to compare the reaction kinetics, rate law and conversion in a batch reactor to the
one in a CSTR system for the same reaction.

The reaction kinetics and rate law of saponification reaction in a CSTR can be
determined using conductivity calibration curve. Conductivity is a measure of how well a
solution can conducts electricity. A solution must contain charged particles, or ions to carry a
current. Most conductivity measurements are made in aqueous solutions, and the ions
responsible for the conductivity come from electrolytes dissolved in the water.

Furthermore, there are two ways to calibrate conductivity sensors. The sensor can be
calibrated against a solution of known conductivity or it can be calibrated against a previously
calibrated sensor and analyzer. Normally, the sensor should be calibrated at a point near the
midpoint of the operating range calibration changes the cell constant. For this experiment, the
calibration curve is prepared using different molar concentration of sodium hydroxide and
sodium acetate.

4
 3.0 LITERATURE REVIEW / THEORY
A type of reactor used commonly in industrial processing is continuous stirred tank
reactor (CSTR) or vat and used primarily for homogeneous liquid-phase flow reactions,
where constant agitation is required. Based on H. Scott Fogler, Elements of Chemical
Reaction, CSTR normally operates at steady state and is assumed to be perfectly mixed.
Consequently, there is no time dependence or position dependence of the temperature, the
concentration or the rate inside the CSTR. As a whole, the reactor was stirred continues
mixed perfect and there is no distinction in the overall density and temperature in the reactor.
This assumption may be made namely the concentration and temperature is identified in all
regions of the reactor is equal to the temperature and density at the reactor output. Another
advantage of this continuous stirred is a reactor of this type has the ability to escort the
temperature and pressure.

4.0 THEORY
Saponification between sodium hydroxide (NaOH, denotes as A) and ethyl acetate
(EA, denotes as B) is basically second order elementary reaction. For steady state constant
volume isothermal CSTR, the design equation is: 
VCA 0 X
V=
−rA

Where V is the reactor volume, X is the reactant and v is the total volumetric flow rate feeds
into the reactor.
For elementary-bimolecular second order reaction, the rate equation is:
-rA=kCACB

Basically, reactant conversion, X, can be calculated using the following equation:

CA
X=1-
CA 0
CB
X=1 -
CB 0

5
The design equation of CSTR also can be written in terms of initial concentrations, reactant
conversion, and reactor volume and feed flow rate. Thus, we need to use the relations: 
CA=CA0 (1-X)
CB=CB0 (1-X) =CA0 (1-X), when CB0= CA0

Therefore, 
-rA=kCA02 (1-X)2
If we combine the above equation, we see that 
vC A 0 X
V=
kC A 0 2(1−X )2
And further simplified to
vC A 0 X
V=
kC A 0(1−X ) 2

6
5.0 METHODOLOGY
1. Conductivity calibration curve is prepared using three points:

i. X = 0.0, use 10mL 0.1M NaOH.

ii. X = 0.5, use a mixture of 5 mL 0.05M NaOH and 5 mL 0.05M
sodium acetate.
iii. X = 1.0, use 10 mL 0.1M sodium acetate.

2. All the valves were closed.

3. 9L solution of 0.1M NaOH (8g per 2L H2O) and 9L solution of 0.1M EA
(19.6mL per 2L H2O) were prepared and these solutions were poured
into tanks T1 and T2 respectively.
4. Next, pumps P1 and P2, and stirrer S1 were switched on. The feed flow rates into the
CSTR were adjusted to be at 40 cm3/min using valves F1 and F2. The stopwatch was
started immediately as the pumps and stirrer were switched on. The conductivity and
temperature of the reaction medium in the CSTR were measured for every 2 minutes
for over 30 minutes.
5. When liquid level inside the CSTR reached 2000 cm3 (2L), the space time,
conductivity and temperature of the reaction medium were recorded.
6. Then, the reaction was flowed into the buffer tank by opening valve V3.

Measurements were continued taken for 10 minutes.

7. Then, valves F1 and F2 were closed, and pumps P1 and P2 were stopped. All liquids
were discharged through valve V4.
8. The experiment was repeated for different feed flow rates at 60 cm3, 100 cm3 and 120
cm3/min.
9. All residual NaOH and Ethyl Acetate were discharged once the experiments were
complete.
10. The pilot plant was cleaned up.

7
6.0 RESULT

Table 1. Calibration Data

0.05M NaOH
Calibration 0.1M Sodium
0.1M NaOH +
Data Acetate
0.05M Sodium
Acetate

Conversion 0.0 0.5 1.0

Conductivity
10,200 2,540 1,160
(μS)

Conductivity Calibration Curve

1.2

0.8
f(x) = − 0 x + 0.96
Conversion

0.6

0.4

0.2

0 Conductivity
1 1

Figure 1

8
Table 2. Experimental Data: Flow Rate = 40cm3/min

Time Conductivit Temp Conversio

CA CB Cc CD 1/Ca
,t y . n
(min (mol/L (mol/L (mol/L (mol/L
(μS) (oC) (mol) (L/mol)
) ) ) ) )
0.0068 0.0068 0.0931 0.0931 146.627
0 300 25.3 0.9318
2 2 8 8 6

0.0073 0.0073 0.0926 0.0926

2 350 26.1 0.9268 136.612
2 2 8 8

0.0155 0.0155 0.0844 0.0844 64.3500

4 1172 26.8 0.8446
4 4 6 6 6

0.0271 0.0271 0.0728 0.0728 36.8731

6 2330 27 0.7288
2 2 8 8 6

0.0456 0.0456 0.0543 0.0543 21.9202

8 4180 27 0.5438
2 2 8 8 1

0.0444 0.0444 0.0555 0.0555 22.5123

10 4060 27.1 0.5558
2 2 8 8 8

0.0432 0.0432 0.0567 0.0567 23.1374

12 3940 27.1 0.5678
2 2 8 8 4

0.0420 0.0420 0.0579 0.0579 23.7981

14 3820 27.1 0.5798
2 2 8 8 9

0.0412 0.0412 0.0587 0.0587 24.2600

16 3740 27.1 0.5878
2 2 8 8 7

0.0412 0.0412 0.0587 0.0587 24.2600

18 3740 27.1 0.5878
2 2 8 8 7

0.0384 0.0384 0.0615 0.0615 26.0281

20 3460 27.1 0.6158
2 2 8 8 1

0.0392 0.0392 0.0607 0.0607

22 3540 27.1 0.6078 25.4972
2 2 8 8
3670 27.1 0.5948 0.0405 0.0405 0.0594 0.0594 24.6791

9
 24
2 2 8 8 7

0.0420 0.0420 0.0579 0.0579 23.7981

26 3820 27.1 0.5798
2 2 8 8 9

0.0434 0.0434 0.0565 0.0565 23.0308

28 3960 27.1 0.5658
2 2 8 8 6

0.0436 0.0436 0.0563 0.0563 22.9252

30 3980 27.1 0.5638
2 2 8 8 6

CA: concentration of NaOH

CB: concentration of EA

CC: concentration of sodium acetate

CD: concentration of ethyl alcohol

1/CA vs Time for v0 = 40cm3/min

160
140
120
1/CA (L/mol

100
80
60
40
20
0
0 10 20 30 40 50 60

Time, t (min)

Figure 2

10
 Table 3. Experimental Data: Flow Rate = 60cm3/min

                 
Time Conductivit Temp Conversio
CA CB CC CD 1/CA
,t y . n
                 
(mol/L (mol/L (mol/L (mol/L
(min) (μS) (oC) (mol) (L/mol)
) ) ) )
                 
0.0289 0.0289 0.0710 0.0710 34.5781
0 2510 27 0.7108
2 2 8 8 5
0.0357 0.0357 0.0642 0.0642 27.9955
2 3190 27.2 0.6428
2 2 8 8 2
4 0.0398 0.0398 0.0601 0.0601 25.1130
3600 27.3 0.6018
2 2 8 8 1
0.0712 0.0712 0.0287 0.0287
6 6740 27.4 0.2878 14.041
2 2 8 8
0.0663 0.0663 0.0336 0.0336 15.0784
8 6250 27.5 0.3368
2 2 8 8 1
0.0635 0.0635 0.0364 0.0364 15.7430
10 5970 27.5 0.3648
2 2 8 8 7
12 0.0631 0.0631 0.0368 0.0368 15.8428
5930 27.5 0.3688
2 2 8 8 4
0.0615 0.0615 0.0384 0.0384 16.2548
14 5770 27.5 0.3848
2 2 8 8 8

11
16 5630 27.5 0.3988 0.0601 0.0601 0.0398 0.0398 16.6334
2 2 8 8
0.0590 0.0590 0.0409 0.0409 16.9434
18 5520 27.6 0.4098
2 2 8 8 1
20 0.0583 0.0583 0.0416 0.0416 17.1467
5450 27.6 0.4168
2 2 8 8 8
0.0579 0.0579 0.0420 0.0420 17.2651
22 5410 27.6 0.4208
2 2 8 8 9
0.0579 0.0579 0.0420 0.0420 17.2651
24 5410 27.6 0.4208
2 2 8 8 9
26 5370 27.6 0.4248 0.0575 0.0575 0.0424 0.0424 17.3852
2 2 8 8 6

CA: concentration of NaOH

CB: concentration of EA

CC: concentration of sodium acetate

CD: concentration of ethyl alcohol

1/CA vs Time for v0 = 60cm3/min

40

35

30

25
1/CA (L/mol

20

15

10

0
0 5 10 15 20 25 30 35 40 45

Time, t (min)

Figure 3

12
 Table 4. Experimental Data: Flow Rate = 100cm3/min

                 
Time Conductivit Temp
Conversion CA CB CC CD 1/Ca
,t y .
                 
(min) (μS) (oC) (mol) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
                 
0.05943 0.05943 0.0669
0 2920 27.3 0.6698 0.06698 16.82482
6 6 8
0.05169 0.05169 0.0712
2 2490 27.2 0.7128 0.07128 19.34386
6 6 8
4 0.15087 0.15087 0.0161
8000 27.5 0.1618 0.01618 6.627959
6 6 8
0.14349 0.14349 0.0202
6 7590 27.6 0.2028 0.02028 6.968835
6 6 8
0.13215 0.13215 0.0265
8 6960 27.6 0.2658 0.02658 7.566815
6 6 8
0.13755 0.13755 0.0235
10 7260 27.7 0.2358 0.02358 7.269766
6 6 8
12 0.13683 0.13683 0.0239
7220 27.7 0.2398 0.02398 7.308018
6 6 8
0.13557 0.13557 0.0246
14 7150 27.7 0.2468 0.02468 7.375937
6 6 8

13
16 7140 27.7 0.2478 0.13539 0.13539 0.02478 0.0247 7.385743
6 6 8
0.13683 0.13683 0.0239
18 7220 27.7 0.2398 0.02398 7.308018
6 6 8
0.13791 0.13791 0.0233
20 7280 27.8 0.2338 0.02338 7.25079
6 6 8
0.13773 0.13773 0.0234
22 7270 27.8 0.2348 0.02348 7.260266
6 6 8

0.14223 0.14223 0.0209

24 7520 27.8 0.2098 0.02098 7.030569
6 6 8

CA: concentration of NaOH

CB: concentration of EA

CC: concentration of sodium acetate

CD: concentration of ethyl alcohol

1/CA vs Time for v0 = 100cm3/min

25

20

15
/CA (L/mol

10

0
0 5 10 15 20 25 30 35 40 45

Time, t (min)

Figure 4

14
 Table 5. Experimental Data: Flow Rate = 120cm3/min

                 
Time Conductivit Temp
Conversion CA CB CB CD 1/Ca
,t y .
                 
(min) (μS) (oC) (mol) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
                 
0 4170 27.4 0.5448 0.04552 0.04552 0.05448 0.05448 21.96837

2 8750 27.5 0.0868 0.09132 0.09132 0.00868 0.00868 10.9505

4
8920 27.6 0.0698 0.09302 0.09302 0.00698 0.00698 10.75038

6 8670 27.7 0.0948 0.09052 0.09052 0.00948 0.00948 11.04728

8 7830 27.7 0.1788 0.08212 0.08212 0.01788 0.01788 12.1773

10 7600 27.7 0.2018 0.07982 0.07982 0.02018 0.02018 12.52819

12
8150 27.7 0.1468 0.08532 0.08532 0.01468 0.01468 11.72058

14 8070 27.8 0.1548 0.08452 0.08452 0.01548 0.01548 11.83152

15
 16 7950 27.8 0.1668 0.08332 0.08332 0.01668 0.01668 12.00192

18 7030 27.8 0.2588 0.07412 0.07412 0.02588 0.02588 13.49164

20 6210 27.8 0.3408 0.06592 0.06592 0.03408 0.03408 15.1699

22 5480 27.8 0.4138 0.05862 0.05862 0.04138 0.04138 17.05902

24 5630 27.8 0.3988 0.06012 0.06012 0.03988 0.03988 16.6334

CA: concentration of NaOH

CB: concentration of EA

CC: concentration of sodium acetate

CD: concentration of ethyl alcohol

1/CA vs Time for v0 = 120cm3/min

25

20

15
1/CA (L/mol

10

0
0 5 10 15 20 25 30 35 40 45

Time, t (min)

Figure 5

16
Table 6. Experimental Data: Space Time

Flow Rate Space Time Conductivity Temp. Conversion

υo τ T X

(cm3/min) (min) (μS) (oC)

40 28 3960 27.1 0.57

60 17 5450 27.6 0.42

17
100 13 7170 27.7 0.24

120 12 8130 27.8 0.15

18
Calculation
Based on Figure 1 the conductivity calibration curve, we get the linear equation of the curve
as y = -1x10-4x +0.9618, where y represents conversion value, x represents conductivity (μS).

When flow rate is 40 cm^3/min, the conductivity at time, t=10min is 4060 μS, the conversion
value is y = -1E-4(4060) + 0.9618

= 0.5558

For the concentration of NaOH after the reaction,

= (1 - X)

= 0.1 M (1 –0.5558)

= 0.04442 M

= 0.04442 mol/L

For the concentration of Ethyl Acetate,

=0.04442 mol/L

For the concentration of Sodium Acetate,

= .X

= 0.1M (0.5558)

= 0.05558 M

= 0.05558 mol/L

For the concentration of Ethyl Alcohol,

= 0.05558 mol/L

19
Four linear graphs of 1/CA vs. time are plotted, which indicates the second order reaction of
the saponification process.

1/CA =1/CA0 + kt

By using graphical method, we know that the slope of the graph indicates the value of k.
Average value of k based on the four graphs (of different flow rates) kav=
(2.8246+0.4154+0.3185+0.0618)/4

= 0.9051 L/mol.min

Whereas by using analytical method, from the equation simplified

V= , k=

At v0 = 40 cm3/min, V= 2000cm3, X = 0.57980, CA0 = 0.1mol/L

40 (0.57980)
k =
2000(0.1)(1−0.57980)2

=0.6567 L/mol.min

So the value of k average using analytical method,

0.6567+0.6002+0.5925+0.7245
K=
4

=0.6435 L/mol.min

Theoretical Space time, τth can be calculated through the equation below:

τ = V/v0

where V is volume of reactor and v0 is the volumetric flow rate entering the reactor.

For flow rate v0 = 40 cm3/min, because there are two reactants flowing in the reactor
with the same flow rate, thus we use v0 = 2(40) = 80 cm3/min.

= 25 min

20
7.0 DISCUSSION

At the end of our experiment and after done the calculation, we can calculate the
reactant conversion, verify the reaction order and determine the rate constant.
Based on the graph 1 which is graph of conversion against conductivity of three
different concentrations of reactants or known as conductivity calibration curve, we get
the linear equation of the curve as y = = -1x10-4x + 0.9618, where x represents as
conductivity and y represents as reactant conversion. The conductivity calibration curve
represents the conversion-conductivity relationship of the reaction mixture and provides
a mean to get concentration versus time data. Hence, we can calculate the value of the
conversion at every minute and followed the calculation to find concentration sodium
hydroxide (CA), ethyl acetate (CB), sodium acetate (CC) and ethyl alcohol (CD) based on
the formula: 1/CA =1/CA0 + kt .
By using graphical method which is concentration versus time graph, we know
that the slope of the graph indicates the value of rate constant of saponification reaction
between sodium hydroxide and ethyl acetate. Hence the average value of rate constant
based on the four different flow rate is 0.9051 L/mol.min. Whereas by using analytical
method based on the equation, the average value of rate constant is 0.6435 L/mol.min.
From these two different values we found that the value of rate constant k by using
graphical method is lower than by using the design equation of CSTR due to several
factors.
Overall, the theoretical space time is higher than experimental due to some error
during taken the space time. Unfortunately, we are late recorded the space time because
we are not clearly see either the liquid reach the valve V3 or not. Saponification
between sodium hydroxide and ethyl acetate is basically second order elementary
reaction. It is proved by our graph respect to reaction between sodium hydroxide and
ethyl acetate since graph 1/CA versus time is a linear graph which is corresponding to
the second order and the slope of the graph referring to the positive rate of constant.

21
Comparison between batch reactor and CSTR in term of reaction kinetics, rate law
and conversion for the same reaction:
Batch Reactor CSTR
Reaction kinetics Both reactors will process the reaction at the same speed
Rate Law Both reactors have the same rate law which is second order. Rate
law is independent of type of reactors used.
Conversion Conversion increases with the time Time usually increases
spent in the reactor. The longer with the increasing reactor
reactant stays in the reactor, the more volume. The bigger/longer
the reactant is converted to product the reactor, the more time it
until reach equilibrium. will take the reactants to
flow completely through
the reactor and more time
to react

Error during the experiment:

1. Conductivity meter switch off by itself when the reading was taken.

2. Error occurs during preparation of the solutions.

3. Flow rate does not consistent during a time. It goes up and down by itself.

4. Have side reaction during the experiment.

5. Our reaction was initially too dilute maybe.

6. Possible error within the conductivity meter.

7. The solution in both tank reactor A and B was leaked and spilled out.

Recommendations for future work:

22
1. Always adjusted the flow rate so that the flow was consistent.

2. Always take noted on conductivity meter so that when it is switch off by itself,
we already have the reading.

3. Become familiar with the analytical equipment.

4. Do research before entering the lab and do the experiment.

5. Split up the task for each person to do during lab prior to running the
experiment.

23
 8.0 CONCLUSION
Continuous-stirred tank reactor (CSTR), is a widely used reactor in industrial
processing which is used primarily for liquid phase reaction. Commonly, it is operated at
steady state and assumed to be perfectly mixed. By using different molar concentration of
sodium hydroxide and ethyl acetate, the conductivity calibration curve is prepared. This
calibration curve can be used to determine the reaction kinetics and the rate law of the
process. Based on the graph concentration versus time, we get the value of rate constant
which is in this experiment we get k = 0.9051 L/mol.min and little bit differ by using by
formula which is k = 0.6435 L/mol.min. Apart from that, the reaction order is successfully
approved which is second order of reaction based on linear graph of concentration versus
time.

9.0 REFERENCES
1. H. Scott Fogler, “Elements of Chemical Reaction Engineering”, 4th
edition, Pearson Education Limited, 2014.

10.0 APPENDICES

Figures show Continuous stirred tank reactors, (a) With agitator and internal heat
transfer surface, (b) With pump around mixing and external heat transfer surface.

24
 (a)

(b) (c)

The figures show the (a) zero order reaction (b) first order reaction (c) second order
reaction

25