TABLE OF CONTENT

NUM CONTENTS PAGE

1.0 Abstract 1

2.0 Introduction 2

3.0 Theory/Literature Review 4

4.0 Methodology 6

5.0 Results And Discussion 7

6.0 Conclusion 17

7.0 References 17

8.0 Appendices 17
1.0 ABSTRACT

The experiment aims to study the saponification reaction of sodium hydroxide

an ethyl acetate in a ContinuousStirred Tank Reactor (CSTR). In this experiment,
the aims also include investigating the operational behaviour of a reaction in the
CSTR system, techniques when using CSTR for a reaction process and effect of
flow changes on the reaction. Before all apparatus is set-up, the conductivity
calibration curve with different molar concentration were prepared to determine
the conversion of the reactants to products in the reactor since we cannot
distinguish the mixture of reactants and products easily from the mixture. Then,
both sodium hydroxide and ethyl acetate were prepared according to the given
volume and concentration before transferred to the tanks. When the process
starts, the conductivity and temperature of the reaction were recorded in every
two minutes for 30 minutes. When the liquid level in the CSTR reached 2L, the
space time as well as conductivity and temperature was recorded. After flow the
reaction medium into the buffer tank, the readings are recorded for another 10
minutes. Then, all valves and pumps were closed, and all liquid will be discarded
through valve V4. The process is repeated several times using different feeds of
flow rates. Theoretically, as the time goes once the experiment starts, the conductivity
values should gradually close up its value to the conductivity value of pure product that is
determined before the reaction starts. The conversion should gradually increase as the time
goes by. From the result obtained, it shows that on the graph concentration versus time, we
get the value of rate constant which is in this experiment we get k = 0.6342 L/mol. min and
little bit differ by using by formula which is k = 1.317 L/mol .min. Other than that, the
reaction order is successfully to approve which 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.
2.0 INTRODUCTION

The Continuous- Stirred Tank Reactor (CSTR) is common type of reactor used
in industrial processing which is primarily used for liquid phase reaction. The
reactor was operate in steady state condition with continuous flow of reactants
and products and assumed as perfectly mixed. The feed assumes a uniform
composition throughout the reactor; exit stream has the same composition as in
the tank. There is no time dependence or position dependence of the
temperature, the concentration and the reaction rate in the tank. The usage of
the CSTR is when agitation is required and series configurations for different
concentration streams. Besides that, the advantages using this reactor compare
to the other are it has good temperature control, easily adapt to two phases, low
operating cost and easy to clean. But, the CSTR has lowest conversion per unit
volume and requires large volume to obtain the desired conversions. When high
conversions of reactants are needed, several CSTRs in series can be used.
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. Beside 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
significant 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. The result of CSTR of the reaction kinetics,
rate law and conversion is compared with a batch reactor for the same reaction
as stated in scope of experiment.

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. 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.
3.0 LITERATURE REVIEW

In this experiment we are going to use continuous stirred tank reactor (CSTR)
to react sodium hydroxide and ethyl acetate to produce sodium acetate. Based
on H. Scott Fogler, Elements of Chemical Reaction CSTR normally operated at
steady state and is assumed to be perfectly mixed. Based on this statement, the
temperature of the reactor and reaction mixture should not have any major
change throughout the experiment. Concentration and volume of the reactants
should be the same as another reactant since it is a one-to-one ratio for the
reaction. The reactants are well mixed and so the reaction must be efficient.
However, reactants and products are always mixed well together in the reactor
making it difficult to determine the product conversion. That is why a standard
conductivity calibration curve has to be prepared before the experiment.
Conductivity of the mixture will indicate the percent products present which is
determine using conductivity meter.
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 :

v CA 0 X
V=
r A

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 :

r A=k C A C B

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

CA
X =1
CA 0

CB
X =1
C B0

The design equation of CSTR also can be written in terms of initial

concentrations, reactant conversion, reactor volume and feed flow rate. Thus, we
need to use the relations :

C A =C A 0 ( 1X )

C B=C B 0 ( 1 X )=C A 0 (1X ) , when

C B 0=C A 0

Therefore,

r A=k C 2A 0 (1X )2

If we combine the above equation, we see that

 v CA 0 X
V=
k C 2A 0 (1 X)2

And further simplified to

vX
V=
k C (1 X)2

A0
4.0 METHODOLOGY

A. Calibration graph plot

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 NaOH and 5 mL sodium acetate

iii. X = 1.0, use 10 mL 0.1M sodium acetate

B. Operating procedure

1. 9L solution of 0.1M NaOH (8g per 2L H2O) and 9L solution of 0.1M EA

(19.6mL per 2L H2O) are prepared and these solutions were poured into
tanks T1 and T2 respectively.
2. Next, pumps P1 and P2, and stirrer S1 are switched on. The feed flow rates
into the CSTR are adjusted to be at 40 cm 3/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.
3. When liquid level inside the CSTR reached 2000 cm 3(2L), the space time,
conductivity and temperature of the reaction medium were recorded.
4. Then, the reaction is flowed into the buffer tank by opening valve V3.
Measurements were continued taken for 10 minutes.
5. After 30 minutes, valves F1 and F2 were closed, and pumps P1 and P2
were stopped. All liquids were discharged through valve V4.
6. The experiment was repeated for different feed flow rates at 60 cm 3, 100
cm3 and 120 cm3.
7. All residual NaOH and Ethyl Acetate were discharged once the
experiments were done.
8. The pilot plant was cleaned up.
 0.05M NaOH +
Callibration 0.05M Sodium 0.1M Sodium
Data 0.1M NaOH Acetate Acetate
Conversion 0.0 0.5 1.0
Conductivity
(S) 12.17 8.69 5.17

5.0 RESULTS AND DISCUSSION

RESULT
Table 1: Calibration Data

Conductivity Calibration Curve

1.2

1
f(x) = - 0.14x + 1.74
0.8 R = 1

0.6
Conversion
0.4

0.2

0
4 5 6 7 8 9 10 11 12 13

Conductivity (S)

Figure 1: Graph of Conversion against Conductivity of three different concentrations of

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

Time, t Conductivity Temperature CA CB CC CD 1/CA

Conversion
(min) (S) (C) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
0 10.75 28.5 0.2033 0.07967 0.07967 0.02033 0.02033 12.55
- -
2 18.27 30.2 -0.8713 0.18713 0.18713 0.08713 0.08713 5.34
- - -
4 4.96 30.0 1.0307 0.00307 0.00307 0.10307 0.10307 325.56
6 7.38 30.0 0.6849 0.03151 0.03151 0.06849 0.06849 31.74
8 9.30 30.0 0.4105 0.05895 0.05895 0.04105 0.04105 16.96
10 9.14 30.0 0.4334 0.05666 0.05666 0.04334 0.04334 17.65
12 9.06 30.1 0.4448 0.05552 0.05552 0.04448 0.04448 18.01
14 8.95 30.1 0.4605 0.05395 0.05395 0.04605 0.04605 18.54
16 8.89 30.1 0.4691 0.05309 0.05309 0.04691 0.04691 18.84
18 8.79 30.2 0.4834 0.05166 0.05166 0.04834 0.04834 19.36
20 8.73 30.2 0.4920 0.05080 0.05080 0.04920 0.04920 19.68
22 8.66 30.2 0.5020 0.04980 0.04980 0.05020 0.05020 20.08
24 8.58 30.3 0.5134 0.04866 0.04866 0.05134 0.05134 20.55
26 8.56 30.3 0.5163 0.04837 0.04837 0.05163 0.05163 20.67
28 8.50 30.3 0.5249 0.04752 0.04752 0.05249 0.05249 21.05
30 8.46 30.3 0.5306 0.04694 0.04694 0.05306 0.05306 21.30
32 8.44 30.3 0.5334 0.04666 0.04666 0.05334 0.05334 21.43

CA: Concentration of NaOH

CB: Concentration of Ethyl Acetate
CC: Concentration if Sodium Acetate
CD: Concentration of Ethyl Alcohol

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

Time, t Conductivity Temperature CA CB CC CD 1/CA

Conversion
(min) (S) (C) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
- - 0.1245
0 -40.81
3.46 30.6 1.2451 0.02451 0.02451 0.12451 1
0.0340
2 0.06595 15.16
9.79 30.8 0.3405 0.06595 0.03405 5
0.0373
4 0.06266 15.96
9.56 30.7 0.3734 0.06266 0.03734 4
0.0440
6 0.05595 17.87
9.09 30.7 0.4405 0.05595 0.04405 5
0.0450
8 0.05495 18.20
9.02 30.7 0.4505 0.05495 0.04505 5
0.0480
10 0.05194 19.25
8.81 30.7 0.4806 0.05194 0.04806 6
0.0510
12 0.04894 20.43
8.60 30.7 0.5106 0.04894 0.05106 6
0.0542
14 0.04580 21.83
8.38 30.8 0.5420 0.04580 0.05420 0
0.0559
16 0.04409 22.68
8.26 30.8 0.5591 0.04409 0.05591 1
 0.0570
18 0.04294 23.29
8.18 30.8 0.5706 0.04294 0.05706 6
0.0590
20 0.04094 24.43
8.04 30.8 0.5906 0.04094 0.05906 6
0.0596
22 0.04037 24.77
8.00 30.8 0.5963 0.04037 0.05963 3
0.0602
24 0.03980 25.13
7.96 30.9 0.6020 0.03980 0.06020 0

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

Time, t Conductivity Temperature CA CB CC CD 1/CA
Conversion
(min) (S) (C) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
- - 0.1125
0 4.30 31.1 1.1250 0.01250 0.01250 0.11250 0 -79.98
0.0296
2 10.10 31.0 0.2962 0.07038 0.07038 0.02962 2 14.21
0.0449
4 9.03 31.0 0.4491 0.05509 0.05509 0.04491 1 18.15
0.0393
6 9.42 31.0 0.3934 0.06066 0.06066 0.03934 4 16.48
0.0446
8 9.05 31.0 0.4463 0.05537 0.05537 0.04463 3 18.06
0.0486
10 8.77 31.0 0.4863 0.05137 0.05137 0.04863 3 19.47
0.0510
12 8.60 31.0 0.5106 0.04894 0.04894 0.05106 6 20.43
0.0522
14 8.52 31.0 0.5220 0.04780 0.04780 0.05220 0 20.92
0.0529
16 8.47 31.0 0.5291 0.04709 0.04709 0.05291 1 21.24
0.0534
18 8.43 31.0 0.5349 0.04651 0.04651 0.05349 9 21.50

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

Time, t Conductivity Temperature CA CB CC CD 1/CA

Conversion
(min) (S) (C) (mol/L) (mol/L) (mol/L) (mol/L) (L/mol)
- - 0.1316
0 2.96 31.0 1.3165 0.03165 0.03165 0.13165 5 -31.59
0.0409
2 9.31 31.0 0.4091 0.05909 0.05909 0.04091 1 16.92
0.0499
4 8.68 30.9 0.4991 0.05009 0.05009 0.04991 1 19.97
0.0544
6 8.36 30.9 0.5449 0.04551 0.04551 0.05449 9 21.97
0.0590
8 8.04 30.9 0.5906 0.04094 0.04094 0.05906 6 24.43
 0.0610
10 7.90 30.9 0.6106 0.03894 0.03894 0.06106 6 25.68
0.0613
12 7.88 30.9 0.6134 0.03866 0.03866 0.06134 4 25.87
0.0626
14 7.79 30.9 0.6263 0.03737 0.03737 0.06263 3 26.76
0.0639
16 7.70 30.9 0.6392 0.03608 0.03608 0.06392 2 27.71
0.0644
18 7.66 30.9 0.6449 0.03551 0.03551 0.06449 9 28.16

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

70.00
20.00 f(x) = 2.74x - 45.06
-30.00 0 R = 0.11
5 10 15 20 25 30 35
-80.00
1/CA (L/mol) -130.00
-180.00
-230.00
-280.00
-330.00

Time, t (min)

Figure 2: Graph of 1/CA against Timefor v0 = 40cm3/min

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

30.00
f(x) = 1.39x - 0.64
20.00
R = 0.39
10.00
0.00
1/CA (L/mol) -10.00 0 5 10 15 20 25 30
-20.00
-30.00
-40.00
-50.00

Time, t (min)

Figure 3: Graph of 1/CA against Time for v0 = 60cm3/min

 1/CA vs Time for v0 = 100cm3/min
40.00
f(x) = 3x - 17.94
20.00
R = 0.34
0.00
-20.00 0 2 4 6 8 10 12 14 16 18 20
1/CA (L/mol)
-40.00
-60.00
-80.00
-100.00

Time, t (min)

Figure 4: Graph of 1/CA against Timefor v0 = 100cm3/min

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

40.00
30.00 f(x) = 2x + 0.58
R = 0.45
20.00
10.00
1/CA (L/mol) 0.00
-10.00 0 2 4 6 8 10 12 14 16 18 20
-20.00
-30.00
-40.00

Time, t (min)

Figure 5: Graph of 1/CA against Time for v0 = 120cm3/min

Table 6: Experimental Data for Space Time

Flow Space Conductivity Temperature, Conversion Theoretical

Rate, v0 time, (S) T (C) k space time,
(cm3/min) (min) (L/mol. th(min)
 min)

40 22.40 8.64 30.2 0.5048 0.4117 25.00

60 14.00 8.38 30.8 0.5420 0.5168 16.67
100 8.51 8.91 31.0 0.4663 0.3274 10.00
120 6.47 8.28 30.9 0.5563 0.5651 8.33
CALCULATION

Based on Graph 1 the conductivity calibration curve, we get the linear equation of the curve
as y = -0.1429x + 1.7395, where

y represents conversion value, X

x represents conductivity (S).

When flow rate is 40 cm3/min, the conductivity at time, t=10 min is 9.14 S,
the conversion value is
y = -0.1429(9.14) + 1.7395
= 0.4334

For the concentration of NaOH after the reaction, CA

CA = CA0 (1 - X)
= 0.1 M (1 0.4334)
= 0.05666 M
= 0.05666 mol/L

For the concentration of Ethyl Acetate, CB

CB = C A
= 0.05666 mol/L

For the concentration of Sodium Acetate, CC

CC = CAO.X
= 0.1M (0.4334)
= 0.04334 M
= 0.04334 mol/L
For the concentration of Ethyl Alcohol, CD
CD = C C
= 0.04334 mol/L

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= (2.7364+1.3881+2.9988+2.0007)/4
= 9.124/4
= 2.281 L/mol.min

Whereas by using analytical method, from the equation simplified

v0 X
V= k C (1X )2
A0

v0 X
k= V C A 0 (1 X)2

At v0 = 40 cm3/min, V= 2000cm3, X = 0.5048, CA0 = 0.1mol/L

40(0.5048)
k = 2000 (0.1)(10.5048)2

= 0.4117 L/mol.min

So the value of k average using analytical method,

kav= (0.4117+0.5168+0.3274+0.5651)/4
= 1.8210/4
= 0.4553 L/mol.min

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

= V/v0

whereV 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.
2000 cm 3
th = 80 cm3/min

= 25 min
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 = -0.0621x +1.1918, 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 (C A), ethyl
acetate (CB), sodium acetate (CC) and ethyl alcohol (CD).

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 0.6342
L/mol.min. Whereas by using analytical method based on the equation, the
average value of rate constant is 1.317 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/C A 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.

Comparison between batch reactor and CSTR in term of reaction

kinetics, rate law and conversion for the same reaction:

Batch Reactor CSTR

Reaction Both reactors will process the reaction at the same speed
kinetics

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 usually increases

time spent in the reactor. The with the increasing
longer reactant stays in the reactor volume. The
reactor, the more the reactant bigger/longer the
is converted to product until reactor, the more time
reach equilibrium. it will take the
reactants to flow
completely through the
reactor and more time
to react

Some errors in the process of experiment include errors during preparation of the solutions,
side reaction occurs during the experiment and inconsistency of flow rates from tanks to
CSTR reactor. The flow rate went up and down due to possibly faulty valve since another
valve from another tank was working fine.

Some recommendations to improve the result include study the experiment before entering
the lab to conduct the experiment and always check for errors before starting the experiment
including preparation of reactants material (weighing and dissolving in solution) and
systematic errors like zero errors.
6.0 CONCLUSION

A common type of reactor used in industrial processing is the continuous-stirred tank

reactor (CSTR) which is used primarily for liquid phase reaction. It is normally operated at
steady state and assumed to be perfectly mixed. The conductivity calibration curve is
prepared using different molar concentration of sodium hydroxide and ethyl acetate. 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 = 0.6342 L/mol.min and little bit differ by using by
formula which is k = 1.317 L/mol.min. Other than that, the reaction order is successfully to
approve which is second order of reaction based on linear graph of concentration versus time.

7.0 REFERENCES

H. Scott Fogler, Elements of Chemical Reaction Engineering, 4rd edition,

Pearson Education Limited, 2014.
Schmidt, Lanny D. (1998). The Engineering of Chemical Reactions. New York:
Oxford University Press

8.0 APPENDICES

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

(a)
 (b) (c)

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