1.

0 SUMMARY

The purpose of the experiment was to carry out bath saponification reaction between ethyl
acetate and sodium hydroxide (NaOH). The next objective is to determine the effect of
temperature on the extent of conversion. Then, the saponification reaction of ethyl acetate with
sodium hydroxide can be represented by the following stoichiometric equation. The experiment
was began by preparing the solution of sodium hydroxide and ethyl acetate. Then the solution are
mixed with distilled water and poured into the batch reactor where the saponification process
occur. Every 5 minutes, sample are taken from the reactor and taken to measure the conductivity.
The conductivity is taken by using a conductivity meter. This is repeated for another 30 minutes
and for each temperature which is 40°C, 50°C and 60°C. Throughout the experiment, it showed
that as concentration of sodium hydroxide increase, the conductivity increases. Then, when
conversion increase the conductivity increase. As the higher temperature applied in the
experiment, the conversion will decreases. This is because, when the conductivity increase the
temperature decreases. In theory, the conductivity is inversely proportional to the conversion.
Therefore, the higher the temperature, the higher the rate of reaction in this batch reactor. There
were a few possible errors that isthe reading of conductivity might have errors. It maybe effect
the result and graph plotted. This might due to unclean conductivity rod as it is supposed to be
wiped every time a sample being tested using the conductivity rod.

1
2.0 DATA AND RESULTS

TABLE FOR EXPERIMENT 1

Volume of NaOH =3L

Volume of Et(Ac) =3L

Initial concentration of NaOH = 0.1 M

Initial concentration of Et(Ac) = 0.1 M

Temperature = 40ºC

Time Temperature Conductivity Concentration of Conversion,

(min) (ºC) (mS/cm) NaOH, CNaOH (M) X (%)
0 30.0 6.00 0.0140 71.21
5 31.8 5.80 0.0130 74.04
10 32.9 4.43 0.0035 93.41
15 34.2 4.24 0.0021 96.10
20 35.1 4.17 0.0016 97.08
25 35.8 4/18 0.0017 96.95
30 36.4 4.21 0.0019 96.52

2
 TABLE FOR EXPERIMENT 2

Volume of NaOH =3 L

Volume of Et(Ac) =3 L

Initial concentration of NaOH =0.1 M

Initial concentration of Et(Ac) =0.1 M

Temperature =50ºC

Time Temperature Conductivity Concentration of Conversion,

(min) (ºC) (mS/cm) NaOH, CNaOH (M) X (%)
0 37.6 5.97 0.0144 71.63
5 33.7 5.33 0.0098 80.68
10 36.1 4.96 0.0072 85.92
15 38.7 4.63 0.0049 90.58
20 40.6 4.45 0.0036 93.13
25 42.2 4.39 0.0032 93.98
30 43.3 4.32 0.0027 94.97

3
 TABLE FOR EXPERIMENT 2

Volume of NaOH =3 L

Volume of Et(Ac) =3 L

Initial concentration of NaOH =0.1 M

Initial concentration of Et(Ac) =0.1 M

Temperature =60ºC

Time Temperature Conductivity Concentration of Conversion,

(min) (ºC) (mS/cm) NaOH, CNaOH (M) X (%)
0 42.5 7.06 0.0221 56.22
5 36.4 6.73 0.0198 60.89
10 40.3 6.24 0.0163 67.82
15 43.8 6.33 0.0169 66.54
20 46.5 6.27 0.0165 67.39
25 48.7 6.34 0.0170 66.40
30 50.4 6.11 0.0154 66.40

4
3.0 ANALYSIS AND DISCUSSION

Concentration of NaOH vs Conductivity

0.06
Concentration of NaOH (M)

0.05 y = 0.0071x - 0.028

R² = 0.9898
0.04

0.03
Series1
0.02 Linear (Series1)

0.01

0
0 2 4 6 8 10 12
Conductivity

Figure 1

y = mX + c

= 0.0071x - 0.028

Slope = 0.0071

y-axis intercept = -0.028

5
 Conversion (%) vs Conductivity
120

100

80
Conversion (%)

60
Series1

40 Linear (Series1)

20
y = -14.14x + 156.05
R² = 0.9898
0
0 2 4 6 8 10 12
Conductivity

Figure 2

y = mX + c

= -14.14x +156.05

Slope = -14.14

y-axis intercept = 156.05

6
 ln [-dCA/dt] vs ln Ca
10

6
ln [-dCA/dt]

5
y = -2.2375x - 5.5882 4
R² = 0.3661
3

0
-7 -6 -5 -4 -3 -2 -1 0
ln Ca

ln [-dCA/dt] Linear (ln [-dCA/dt])

Figure 3

Slope = -2.2375

y-axis intercept = -5.5882

Order of reaction = α, since ln [-dca/dt] = α ln CA + ln k

Thus, α = slope = -2.2375

Rate constant = k, since ln [-dca/dt] = α ln CA + ln k, thus

Ln k = -5.5882

k = e^(-5.5882)

= 3.742x10-3

Intercept values = x-intercept = -4.27

= y-intercept = -5.5882

7
 Conversion (%) vs Time
120

y = 0.8959x + 75.892
100 R² = 0.7072

y = 0.7416x + 76.145
R² = 0.8761
80
Conversion ()%)

40°C
50°C
60 y = 0.2938x + 60.116
R² = 0.5378 60°C
Linear (40°C)

40 Linear (50°C)
Linear (60°C)

20

0
0 5 10 15 20 25 30 35
Time (min)

Figure 4

For temperature 40°C: For temperature 50°C: For temperature 60°C:

Time Conversion Time Conversion Time Conversion

(min) (%) (min) (%) (min) (%)
0 71.63 0 71.21 0 56.22
5 80.68 5 74.04 5 60.89
10 85.92 10 93.41 10 67.82
15 90.58 15 96.1 15 66.54
20 93.13 20 97.08 20 67.39
25 93.98 25 96.95 25 66.4
30 94.97 30 96.52 30 66.4

8
Based on figure 4, it is shows that when the temperature increase, the conversion will decrease.
This is because, when the conductivity increase the temperature decreases. In theory, the
conductivity is inversely proportional to the conversion. So it is determine that the result obey the
theory. However, the temperature effect the rate of reaction. The higher the temperature, the higher
the rate of reaction. This is because, when the temperature increase, the movement of particles
speed increase and collide into each other. This cause the reaction to increase because the
movement energy of particles increase.

9
For temperature 40°C:

1/Ca vs Time (min)

800

700 y = 19.668x + 79.659

R² = 0.8068
600

500
1/Ca

400
Series1
300
Linear (Series1)
200

100

0
0 5 10 15 20 25 30 35
Time (min)

Figure 5

For temperature 50°C:

1/Ca vs Time (min)

400
y = 10.49x + 53.807
350
R² = 0.9883
300

250
1/Ca

200
Series1
150
Linear (Series1)
100

50

0
0 5 10 15 20 25 30 35
Time (min)

Figure 6

10
For temperature 60°C:

1/Ca vs Time (min)

70
y = 0.5354x + 49.205
60 R² = 0.7094

50

40
1/Ca

Series1
30
Linear (Series1)
20

10

0
0 5 10 15 20 25 30 35
Time (min)

Figure 7

Table: 1/Ca vs Time (min)

Time (min) 1/Ca for 40°C 1/Ca for 50°C 1/Ca for 60°C
0 71.43 69.44 45.25
5 76.92 102.04 50.51
10 258.71 138.89 61.35
15 476.19 204.08 59.17
20 625 277.78 60.61
25 588.23 315.5 58.82
30 526.32 370.37 64.94

Temperature (°C) The rate constant,k from slope: (slope = k)

40 19.6680
50 10.4900
60 0.5354

11
 ln k vs 1/T (K)
4

3.5 y = 18735x - 56.384

R² = 0.8555
3

2.5

2
ln k

1.5 Series1
Linear (Series1)
1

0.5

0
0.00295 0.003 0.00305 0.0031 0.00315 0.0032
-0.5

-1
1/T (K)

Figure 8

ln(k2/k1) = Ea/8.3014 J/mol.K (1/313.15K – 1/323.15K)

ln(10.49/19.668)= Ea/8.3014 J/mol.K (1/313.15K – 1/323.15K)

Ea = 52806.29 J/mol

c = y-intercept

ln A = c

A = e(- 56.384)

= 3.256x10-25 m3/mol.s

12
 The purpose of the experiment was to carry out bath saponification reaction between ethyl
acetate and sodium hydroxide (NaOH). This saponification reaction is to produce soap. The next
objective is to determine the effect of temperature on the extent of conversion. The saponification
reaction of ethyl acetate with sodium hydroxide can be represented by the following stoichiometric
equation:

The theory of scheme is to produce soap in a batch reactor by using ethyl acetate and sodium
hydroxide through saponification process. The experiment was began by preparing the solution of
sodium hydroxide and ethyl acetate. Then the solution are mixed with distilled water and poured
into the batch reactor where the saponification process occur. Every 5 minutes, sample are taken
from the reactor and taken to measure the conductivity. The conductivity is taken by using a
conductivity meter. This is repeated for another 30 minutes and for each temperature which is
40°C, 50°C and 60°C.

Based on figure 1 and 2, a calibration curve is plotted to determine the concentration of sodium
hydroxide vs conductivity, and the conversion vs conductivity respectively. In figure 1, when the
concentration of sodium hydroxide increase, the conductivity increases. For figure 2, when
conversion increase the conductivity increase. The purpose of choosing sodium hydroxide (NaOH)
in order to record data is because sodium hydroxide (NaOH) act as limiting reagent in the reaction.

As for the graph conversion vs time at temperature 40°C, 50°C and 60°C, it is discussed above
which is it shows that when the temperature increase, the conversion will decrease. This is because,
when the conductivity increase the temperature decreases. In theory, the conductivity is inversely
proportional to the conversion. So it is determine that the result obey the theory. However, the
temperature effect the rate of reaction. The higher the temperature, the higher the rate of reaction.
This is because, when the temperature increase, the movement of particles speed increase and
collide into each other. This cause the reaction to increase because the movement energy of
particles increase.

As for graph in figure 5,6 and 7, 1/CA vs time at temperature 40°C, 50°C and 60°C, it can be
overall state that as the 1/CA increases, the time will also increase. This is because, when time
getting longer, the concentration of NaOH which directly the limiting reactant become lower as
13
the NaOH has reduced to form the product which is the soap. Furthermore, in figure 8 when In k
increase the 1/T also increases. It can be conclude that it a second order reaction.

There were a few possible errors that is the reading of conductivity might have errors. It maybe
effect the result and graph plotted. This might due to unclean conductivity rod as it is supposed to
be wiped every time a sample being tested using the conductivity rod.

14
4.0 CONCLUSIONS

The purpose of the experiment was to carry out bath saponification reaction between ethyl acetate
and sodium hydroxide (NaOH). This saponification reaction is to produce soap. The next objective
is to determine the effect of temperature on the extent of conversion.

By plotting a calibration curve in order to determine the concentration of sodium hydroxide vs

conductivity, it can be deduced that when the concentration of sodium hydroxide increase, the
conductivity increases. By plotting a calibration curve in order to determine the conversion vs
conductivity respectively, it can be deduced that when conversion increase the conductivity
increase respectively. As for the graph conversion vs time at temperature, it can be deduced when
the temperature increase, the conversion will decrease. However, the temperature effect the rate of
reaction. The higher the temperature, the higher the rate of reaction. This is because, when the
temperature increase, the movement of particles speed increase and collide into each other. This
cause the reaction to increase because the movement energy of particles increase. As for graph
1/CA vs time at temperature, it can be deduced that as the 1/CA increases, the time will also
increase. Furthermore, in figure 8 when In k increase the 1/T also increases. It can be conclude
that it a second order reaction. Thus, the objectives of this experiment as stated above is
successfully achieved.

4.1 RECOMMENDATIONS

A few steps that can be taken in order to prevent these types of errors from occurring. ,
Experimenters have to focus and be patient for the readings to stabilize before recording any data
in order to prevent physical errors (caused by experiments) from occurring. Moreover, work
together to record data, and not just be dependent on just a team member. Next, , team members
should reconfirm with each other on the results to acquire the readings which best fit in order to
prevent recording the wrong data. Besides that, those who conduct the experiment should read the
lab manual prior to conducting the experiment to prevent conducting a slow process. Not just that
, to avoid unwanted results even before conducting the experiment, each team should request
assistance from available technicians to check whether the experiment is faulty or not. Last but not
least, conductivity rod must be clean where it is supposed to be wiped every time a sample being
tested using the conductivity rod to get the accurate reading.

15
5.0 TUTORIAL

1 .Discuss the advantages and disadvantages of using batch reactor in chemical reaction.

Advantages

1. High conversion per unit volume for one pass

2. Flexibility of operation-same reactor can produce one product one time and a different product
the next

3. Easy to clean

Disadvantages

1. High operating cost

2. Product quality more variable than with continuous operation

3.Difficult in large size-scale product.

2. Determine the effect of temperature on chemical reaction

Particles can only react when they collide. Therefore, as two chemicals react, their molecules
have to collide with each other with sufficient energy for the reaction to take place. This is
collision theory. These two particles will only react if they have enough energy. Increasing the
temperature increases reaction rates because of the disproportionately large increase in the
number of high energy collisions. It is only these collisions (possessing the activation energy for
the reaction) which result in a reaction.

16
3. Write the function of each following component in a batch reactor used in this
component.

 Stirrer
To mix chemicals in the batch reactor.
 Thermocouple
To monitor and act as sensor device in the batch contents temperature.
 Temperature controller
Quick response to heating and cooling loads and proper wall temperature of the batch
reactor.

17
6.0 REFERENCES

18
7.0 APPENDICES

Temperature : 40ºC
Concentration of NaOH, CNaOH (M) : y = mX + c, X: conductivity
y = 0.0071x - 0.028

For 0th min:

y = 0.0071(6.0) - 0.028
= 0.0140 M
For 5th min:
y = 0.0071(5.8) - 0.028
= 0.0130 M
For 10th min:
y = 0.0071(4.43) - 0.028
= 0.0035 M
For 15th min:
y = 0.0071(4.24) - 0.028
= 0.0021 M
For 20th min:
y = 0.0071(4.17) - 0.028
= 0.0016 M
For 25th min:
y = 0.0071(4.18) - 0.028
= 0.0017 M
For 30th min:
y = 0.0071(4.21) - 0.028
= 0.0019 M

19
Temperature : 50ºC
Concentration of NaOH, CNaOH (M) : y = mX + c, X: conductivity
y = 0.0071x - 0.028

For 0th min:

y = 0.0071(5.97) - 0.028
= 0.0144 M
For 5th min:
y = 0.0071(5.33) - 0.028
= 0.0098 M
For 10th min:
y = 0.0071(4.96) - 0.028
= 0.0072 M
For 15th min:
y = 0.0071(4.63) - 0.028
= 0.0049 M
For 20th min:
y = 0.0071(4.45) - 0.028
= 0.0036 M
For 25th min:
y = 0.0071(4.39) - 0.028
= 0.0032 M
For 30th min:
y = 0.0071(4.32) - 0.028
= 0.0027 M

20
Temperature : 60ºC
Concentration of NaOH, CNaOH (M) : y = mX + c, X: conductivity
y = 0.0071x - 0.028

For 0th min:

y = 0.0071(7.06) - 0.028
= 0.0221 M
For 5th min:
y = 0.0071(6.73) - 0.028
= 0.0198 M
For 10th min:
y = 0.0071(6.24) - 0.028
= 0.0163 M
For 15th min:
y = 0.0071(6.33) - 0.028
= 0.0169 M
For 20th min:
y = 0.0071(6.27) - 0.028
= 0.0165 M
For 25th min:
y = 0.0071(6.34) - 0.028
= 0.0170 M
For 30th min:
y = 0.0071(6.11) - 0.028
= 0.0154 M

21
Temperature : 40ºC
Conversion, X (%) : y = mX + c, X: conductivity
y = -14.14x + 156.05

For 0th min:

Y = -14.14(6.0) + 156.05
= 71.21 %
For 5th min:
y = -14.14(5.8) + 156.05
= 74.04 %
For 10th min:
y = -14.14(4.43) + 156.05
= 93.41 %
For 15th min:
y = -14.14(4.24) + 156.05
= 96.10 %
For 20th min:
y = -14.14(4.17) + 156.05
= 97.08 %
For 25th min:
y = -14.14(4.18) + 156.05
= 96.95 %
For 30th min:
y = -14.14(4.21) + 156.05
= 96.52 %

22
Temperature : 50ºC
Conversion, X (%) : y = mX + c, X: conductivity
y = -14.14x + 156.05

For 0th min:

Y = -14.14(5.97) + 156.05
= 71.63 %
For 5th min:
y = -14.14(5.33) + 156.05
= 80.68 %
For 10th min:
y = -14.14(4.96) + 156.05
= 85.92 %
For 15th min:
y = -14.14(4.63) + 156.05
= 90.58 %
For 20th min:
y = -14.14(4.45) + 156.05
= 93.13 %
For 25th min:
y = -14.14(4.39) + 156.05
= 93.98 %
For 30th min:
y = -14.14(4.32) + 156.05
= 94.97 %

23
Temperature : 60ºC
Conversion, X (%) : y = mX + c, X: conductivity
y = -14.14x + 156.05

For 0th min:

Y = -14.14(7.06) + 156.05
= 56.22 %
For 5th min:
y = -14.14(6.73) + 156.05
= 60.89 %
For 10th min:
y = -14.14(6.24) + 156.05
= 67.82 %
For 15th min:
y = -14.14(6.33) + 156.05
= 66.54 %
For 20th min:
y = -14.14(6.27) + 156.05
= 67.39 %
For 25th min:
y = -14.14(6.34) + 156.05
= 66.40 %
For 30th min:
y = -14.14(6.11) + 156.05
= 66.40 %

24
Calculations:
Temperature: 40ºC
ln [-dCA/dt] ln CA
For 0th , ln [-dCA/dt] | = 0.00 ln (0.0140) = -4.27
For 5th, | ln -[-2.0x10-4] | = 8.52 ln (0.0130) = -4.34
For 10th, | ln -[-1.9x10-3] | = 6.27 ln (0.0035) = -5.65
For 15th, | ln -[-2.8x10-4] | = 8.18 ln (0.0021) = -6.17
For 20th, | ln -[-1.0x10-4] | = 9.21 ln (0.0016) = -6.44
For 25th, | ln -[ 2.0x10-5] | = - ln (0.0017) = -6.38
For 30th, | ln -[ 4.0x10-4] | = - ln (0.0019) = -6.27

25