Report On Saponification

Reaction Engineering Lab 1
Experiment 4- Armfield CEB MkII (A)
Date Perofrmed: 03/04/12

Date Due : 24/04/12
Reaction Engineering -Experiment 4 A Page 1

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Table of Content
1. Aim………………………………………………………..3
2. Method……………………….…………………...........….1
3. Calculations and Results…………………………………..2
4. Discussion ……………………………………..………….4
5. Conclusion…………………………..……………………..4

1. Aim
The aim of this experiment is to find the reaction rate constant (k) in a stirred batch
reactor. The experiment A is based on isothermal reaction, which is carried out
below and above the ambient temperature using the Armfield CEB MkII batch
reactor.
2. Method:
The stirred Batch Reactor was already set up for the lab to carry on the experiment
to find the rate constant (k). Check the stirred water circulatory system, adjust the
set point of the temperature controller to 155 C and switch the HEAT/CHILL switch
on the CEX console to chill.
The reaction chosen for the isothermal demonstration is the saponification of ethyl
acetate by sodium hydroxide. Charge the batch reactor with 0.5 litres of the sodium
hydroxide solution. Switch on the agitator and adjust the speed setting to 7.0. As
the experiment involves the collection and storage of conductivity data, the data
output port in the console must be connected to the data logger and the computer as
detailed in the instruction leaflet. This enables conductivity to be recorded at
selected time intervals over a selected period. Collection of data will be carried on
until steady state condition is reached, it take approximately 30 minutes. Also
throughout the experiment the temperature was maintained at 155 C by introducing
ice bag into the chilled water circulatory system.
Now carefully add 0.5 liters of ethyl acetate solution and instigate the data logger
program. The has been determined that the degree of conversion of the reagents
affects the conductivity of the reactor contents so that recordinfg the conductivity
with respect to time using Armfield Data Logger can be used to calculate the
amount of conversion.

3. Calculations and Results:
Nomenclature:
a µ=sodium h yrdoxide concentration∈feed vessel ( molL )=0.05 mol / L

b µ=et h yl acetate concentration∈t h e feed vessel ( molL )=0.05 mol/ L
c µ=sodium acetate concentration∈t h e feed vessel ( molL )=0 mol/ L
T =reactor temperature∈ Kelvin ( K )=286 K
V =reactor volume∈litre ( L )∨cubic decimeter ( d m3 )=1 L
Sample Calculation for t=1 minute :
C ∞=bo if bo>ao
C ∞=ao if bo ≥ ao
At t=0,ao=0.03 M ∧bo=0.03 M
T h erefore , C ∞=0.03 M
1+0.0284 ( T −294 )∗c

Λ ∞=0.070 ¿
Λao=0.195 [1+0.0184 (T −294)]∗ao∗1000=4.13 mS

Λ ∞=0.070 [ 1+0.0284 ( 286−294 ) ]∗0.03∗100=1.39 mS
Ao= Aao ,assume co=0
a ∞=0if ao<bo
a ∞=( ao−bo ) for ao ≥ bo
T h erefore a ∞=0.03−0.03=0
Λ 1=3.26 mS
a 1=( a ∞−ao )
[ Λo− Λ 1
Λo− Λ ∞
+ao
]
¿ ( 0−0.03 )
[ 4.13−3.26
4.13−1.39 ]
+0.03=0.02 M
{ ao−a 1 }
T h erefore , =18.67
{ ao . a 1 }
From the kinetic analysis of a general second order reaction it can be shown that:
−X
k . t=
a ( a−x )
Where k is the reaction rate constant and t is the time of reaction. We know:
X =a 1−ao
Therefore, substituting for X gives:

−ao−a 1
k . t=
ao . a 1

Hence, a plot of k against (ao-a1)/(ao.a1) will give a straight line. The gradient of
the straight line can be used to find k as shown below. Using a regression line, the
equation was determined.
(a0-a1)/(a0.a1) vs time
180.00
160.00 f(x) = 1.49x + 24.84

R² = 0.99
140.00
120.00
100.00 (a0-a1)/(a0.a1)
Linear ((a0-a1)/(a0.a1))
80.00
60.00
40.00
20.00
0.00 Time (minutes)
Figure1.1
Using the results from the experimental data, the concentration of NaOH can be
plotted:

Concentration
0.02
0.02
0.01
0.01
0.01 Concentration
0.01
0.01
0.00
0.00
0.00 Time (minutes)
Figure1.2
Therefore, from the above graphs, the reaction rate constant:

L
k =1.493
mol∗min
Discussion:
From the above calculations we can see that the values of a µ , b µ , c µ , T ∧V can
be obtained from the experiment conditions, by using the above values in the
spreadsheet and applying appropriate formulas given the values of sodium
hydroxide concentration (a1) and sodium acetate concentration (c1) and the degree
of conversion (X) for the values of conductivity taken over a period of the
experiment can be calculated. The data was recorded alongside the conductivity
values and the above graphs (Figure1.1 and Figure1.2) were plotted. The gradient
of the first graph (Figure1.1) give the rate constant (k). The graph of (a0-a1)/

(a0.a1) vs time is not a perfect straight line, therefore the line of best fit was used
to find the gradient.
Initially when the experiment was started, the temperature controller is to be set at
15 5C, and data logger program was started, but the problem was temperature of
this reaction did not remains constant. In this experiment reaction temperature is
maintained by using chilled water, Flow of chilled water is automatically
controlled by temperature controller in the console unit. Then the team recognized
that agitator was not started when the reactants were introduced into the reactor. So
the readings were noted again. And after the agitator was started temperature was
maintained by placing ice bags into the chilled water system.
From the graph (Figure 1.2) it can be seen that concentration of sodium hydroxide
decreases as time increases. Results for the rate constant of this reaction seem
consistent. Some of the errors in this experiment can be, temperature was not
5 accurate amount of the reactants might not be used
accurately maintained at 15 C,
and there might not be perfect mixing by the agitator resulting into the error.
This reaction slowly and gradually progresses towards equilibrium which results
into steady state. Steady state conditions are reached after 30 to 40 minutes of the
experiment has started
5. Conclusion
When we observe the trend of the experiment results, it is concluded that the
results obtained have less errors and therefore has very close accuracy ignoring the
effect of experimental errors. From the trend of the results obtained its noted that
as the temperature increases, the reaction rate increases exponentially.

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Reaction Engineering Lab 1

Experiment 4- Armfield CEB MkII (A)

Date Perofrmed: 03/04/12

Reaction Engineering -Experiment 4 A Page 1

Reaction Engineering -Experiment 4 A Page 2

Reaction Engineering -Experiment 4 A Page 3

a µ=sodium h yrdoxide concentration∈feed vessel ( molL )=0.05 mol / L

V =reactor volume∈litre ( L )∨cubic decimeter ( d m3 )=1 L

Sample Calculation for t=1 minute :

1+0.0284 ( T −294 )∗c

Λao=0.195 [1+0.0184 (T −294)]∗ao∗1000=4.13 mS

Reaction Engineering -Experiment 4 A Page 4

Ao= Aao ,assume co=0

a ∞=( ao−bo ) for ao ≥ bo

Therefore, substituting for X gives:

Reaction Engineering -Experiment 4 A Page 5

160.00 f(x) = 1.49x + 24.84

0.00 Time (minutes)

Reaction Engineering -Experiment 4 A Page 6

0.00 Time (minutes)

Therefore, from the above graphs, the reaction rate constant:

Reaction Engineering -Experiment 4 A Page 7

Reaction Engineering -Experiment 4 A Page 8

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