Laboratory Report Submission Form Reaction Engineering (CKB 20104)

To: Dr Nor Shahirah Mohd Nasir Group No: 7 Week: 6

From: (Student Name) Student ID Number:
1) ANIS BINTI ANIZAM 55216114472
2) NURUL SYAFIQAH BINTI YAHYA 55213114011
3) MUHAMMAD ADAM IBTISAM BIN MUSTAFFA 55214114208
4) FAIZ FAZDLEY BIN MOHD ZAHRI 55214114155
Title of experiment:(Number of Experiment) Date of experiment:
EXPERIMENT 1B : Effect of Temperature on the Batch Saponification Reaction 26 FEBRUARY 2018

Received by: Date Due: 5 MARCH 2018

Dr Nor Shahirah Mohd Nasir

VERY GOOD EXCELLENT

CRITERIA VERY POOR 1 POOR 2 GOOD 3
4 5

1.0 SUMMARY (1 PAGE ONLY) (TOTAL PERCENTAGE, 10%)

STUDENT NAME 1: ANIS BINTI ANIZAM (FILL IN!)
Brief review on the objectives of the experiment, main experimental results and discussion deemed
2 4 6 8 10
significant and conclusions obtained from the work.

2.0 DATA AND RESULTS (TOTAL PERCENTAGE, 10%)

STUDENT NAME 1: ANIS BINTI ANIZAM (FILL IN!) 2 4 6 8 10
1. Data are presented as deemed suitable with complete label and units.
3.0 ANALYSIS AND DISCUSSION (TOTAL PERCENTAGE, 20%)
STUDENT NAME 2: NURUL SYAFIQAH BINTI YAHYA (FILL IN!)
1. Explanations of the referred table and figure are presented after the table and figure.
4 8 12 16 20
2. Discuss on the findings and relations to the theory and objective of experiment.

4.0 CONCLUSIONS AND RECOMMENDATIONS (TOTAL PERCENTAGE, 20%)

STUDENT NAME 3: MUHAMMAD ADAM IBTISAM BIN MUSTAFFA (FILL IN!)
1. Summary of the results to relate the findings or results with the theory applicable to the experimental. 4 8 12 16 20
2. Suggest improvements in apparatus or measurement procedure, or experimental procedures for
future.

5.0 TUTORIAL (TOTAL PERCENTAGE, 20%)

STUDENT NAME 4: FAIZ FAZDLEY BIN MOHD ZAHRI (FILL IN!)
4 8 12 16 20
6.0 REFERENCES & APPENDICES (TOTAL PERCENTAGE, 5%) ALL STUDENT
Attach sample of calculation made in discussion part. 1 2 3 4 5
 STUDENT STUDENT STUDENT STUDENT
SECTION %
1 2 3 4
PRE-LABORATORY ASSESSMENT 5

LABORATORY PSYCHOMOTOR ASSESSEMENT 20

SUMMARY 10

DATA AND RESULTS 10

ANALYSIS AND DISCUSSION 20

CONCLUSIONS AND RECOMMENDATIONS 20

TUTORIAL 20

REFERENCES & APPENDICES (SAME FOR ALL STUDENTS) 5

TOTAL (50%) 50
SUMMARY

This experiment is purposely to study the effect of temperature on the batch saponification reaction
of ethyl acetate and sodium hydroxide in the batch reactor. By using different molar concentration
of sodium hydroxide and ethyl acetate, the conductivity calibration curve is prepared that used to
determine the reaction kinetics and the rate law of the process. By referring to the graph
conversion, X versus reaction time for both 40oC and 50oC, the conversion of the reactant was
increasing. This means that the conductivity of a reaction at 50ºC is higher than 40ºC when there
is more reactant available in the solution. Besides, the rate constant, k value obtained from the
graph is decreasing when the temperature is increased. This experiment is obeying the Arrhenius
theory which the rate constant value is high which 1.1412 at temperature 40 oC and getting low to
0.51 at temperature 50oC. The activation energy obtained at 40oC is -0.1136 KJ/mol whereas at
50oC the activation energy is -0.1164 KJ/mol which means that the activation energy is much
require at 40oC compare to 50ºC. Due to some errors, the result obtained may be affected. There
might be confusing when taking the reading of conversion by using the conductivity meter since
the reading of the temperature keeps on increasing and decreasing. The ionized water used might
have some impurities that cause an error and affect the solution.
 RESULT

Volume of NaOH = 0.5 L

Volume of Et(Ac) = 0.5 L
Initial concentration of NaOH = 0.1 M
Initial concentration of Et(Ac) = 0.1 M
Temperature = 40 C

Table 1: Effect of temperature on the batch saponification.

Concentration of NaOH, Conversion, 𝟏

Time Temperature Conductivity 𝑪𝑨
CNaOH (M) X (%)
(min) (°C) (mS/cm)
(From calibration curve) (Self-calculation) (𝑴−𝟏)
0 40 8.86 0.03305 66.95 30.26
5 40 8.67 0.03205 67.95 31.20
10 40 8.16 0.02902 70.98 34.46
15 40 8.03 0.02810 71.9 35.59
20 40 7.93 0.02750 72.5 36.36
25 40 7.82 0.02650 73.5 37.74
30 40 7.81 0.02649 73.51 37.75
35 40 7.80 0.02648 73.52 37.76
 Volume of NaOH = 0.5 L
Volume of Et(Ac) = 0.5 L
Initial concentration of NaOH = 0.1 M
Initial concentration of Et(Ac) = 0.1 M
Temperature = 50 C

Table 2: Effect of temperature on the batch saponification.

Concentration of NaOH, Conversion, 𝟏

Time Temperature Conductivity 𝑪𝑨
CNaOH (M) X (%)
(min) (°C) (mS/cm)
(From calibration curve) (Self calculation) (𝑴−𝟏)
0 53 7.46 0.02405 75.95 41.58
5 53 7.41 0.02400 76 41.67
10 50 7.34 0.02309 76.91 43.31
15 50 7.34 0.02309 76.91 43.31
20 50 7.34 0.02309 76.91 43.31

Table 3: The value of all the different temperatures, k and 1/T.

Temperature (0C) ln k 1/T

40 0.1321 0.0250
50 -0.6931 0.02
 12
y = 140x + 4
10 R² = 0.9898

Conductivity (ms/cm)
8

0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration of NaOH (M)

Figure 1: Standard calibration NaOH

76
y = 0.9756x + 66.961
74 R² = 0.8564

72
Conversion, X

70

68

66

64

62
0 5 10 15 20 25 30 35
Reaction time, t

Figure 2: Graph of conversion vs reaction time, t at 40°C

 77.2
77 y = 0.283x + 75.687
R² = 0.7625
76.8
76.6
Conversion, X 76.4
76.2
76
75.8
75.6
75.4
75.2
0 5 10 15 20
Reaction time, t

Figure 3: Graph of conversion vs reaction time, t at 50°C

45
40 y = 1.1412x + 30.005
R² = 0.8832
35
30
1/CA (M¯1)

25
20
15
10
5
0
0 5 10 15 20 25 30 35
Reaction rate , t

Figure 4: Graph of 1/CA vs reaction time, t at 40°C

 44
y = 0.51x + 41.106
43.5 R² = 0.7625

43
1/CA (M¯1)
42.5

42

41.5

41

40.5
0 5 10 15 20
Reaction time, t

Figure 5: Graph of 1/CA vs reaction time, t at 50°C

0.2
0.1
0
0.025 0.02
-0.1
-0.2
In K

-0.3
-0.4
-0.5
-0.6
y = -0.8252x + 0.9573
-0.7
R² = 1
-0.8
1/T

Figure 6: Graph of In K vs 1/T

DISCUSSION

For this experiment, there are three main objective which is to measure the rate constant of
the reaction between ethyl acetate and sodium hydroxide under batch condition. Next, to study the
liquid phase reaction kinetics in a batch reactor and to study the effect of temperature on the
reaction in a batch reactor. This experiment was run at 2 different temperature which are 40°C and
50°C. then, the sample were collected every 5 minutes and the conductivity were measured by
using conductivity meter. The result was recorded in table 1 and 2.

Next, the concentration of the NaOH in the reactor was obtained from the calibration curve.
The graph is about the conductivity against the calibration curve of concentration NaOH based on
equation y = 140x + 4, the concentration was calculated. When the value of X for each temperature
was calculated, the conversion X (%) were calculated by using the formula provided in appendix.
There might be some error while preparing the solution that will affect the graph in this experiment.

By referring the graph of conversion, X against time, both temperature showed the
increasing conversion, X of NaOH against the time. The highest conversion for 40°C of
temperature is 73.52 while for 50°C of temperature showed that the highest value if conversion is
76.91. From both graph, it can conclude that the higher the temperature, the higher the conversion
and it followed the theory.

For the second order reaction, the rate law given was calculated to get the value that need
to be used in the graph of 1/𝐶𝐴 against time for both temperature. The graph shows that, when the
temperature increase, the higher the value of the 1/𝐶𝐴 graph. Basically, the result is followed as
the theory stated, which is the higher the temperature, the higher the value of 1/𝐶𝐴 .

In addition, the value ln k against 1/T was plotted in the graph by value that get from the
Arrchenius equation. The graph shows that, the slope were decreasing as the final value of
activation energy was slightly smaller. It might some error has occurred during pouring the
solution. Thus, for 50°C reading, the new NaOH solution was prepared. This will interrupt the
reading of the result.

In conclusion, the graph of this experiment were followed the theory stated for this
experiment.
CONCLUSION

The objective of the experiment were to measure the rate constant of the reaction between
ethyl acetate and sodium hydroxide under batch condition. Next, to study the liquid phase reaction
kinetics in a batch reactor and to study the effect of temperature on the reaction in a batch reactor.
Based on the results obtained and the theory we have, we can conclude that the objective of the
experiment was achieved but there are some important details we must not forget. As the
experiment run in two conditions for determine the difference effect of temperature which when
the operation batch reactor are 40°C and 50°C. As the theory, the higher the temperature, the more
efficient the reaction as the particles are highly collides each other. Next, for the pattern of
conversion of X against time, the highest conversion for 40°C of temperature is 73.52 while for
50°C of temperature showed that the highest value if conversion is 76.91. Moreover, the value of
the 1/𝐶𝐴 graph also increase followed by the increase of temperature. It can concluded that the
results obtained did prove the theory. However, for the value ln k against 1/T was plotted in the
graph shows that the slope were decreasing as the final value of activation energy was slightly
smaller. It might some error has occurred during pouring the solution. Thus, for 50°C reading, the
new NaOH solution was prepared. This will interrupt the reading of the result.

RECOMMENDATION

There were a few recommendations to overcome the errors that might affect the result of
this experiment. As stated in the lab manual, we should have a better equipment when operating
the reactor. Ensuring that both temperatures can ensure that the expected results can be achieved.
Second, we do not think that maintenance right before an experiment was about to be conducted
is good. Because we decide to run the experiment using beaker as an open batch reactor. First, the
raw chemical had to change their scale of concentration and volume. Second, when we operated
in open ractor, the temperature of the reactor will get in interrupt as we working in room
temperature with some quite strong wind from the fan in the lab. The results may not so accurate
as the manual but as long as they follow the theory. By overcoming this problems, we can achieve
a better result in this experiment and thus achieve the theoretical results.
TUTORIAL

1. Describe an example of industrial applications other than saponification that utilized

batch reactors in its process. Discuss the advantages and disadvantages of using batch
reactors in chemical reaction.

Batch processes are suitable for small production and for processes where a range of different
products or grades is to be produced in the same equipment. Examples of processes that use batch
reactors include the manufacture of colorants and margarine. The reactors are also used at
wastewater treatment plants for the activated sludge process, a procedure that uses a wide range of
bacteria to remove contaminants from the water. Last but not least, it is also use in pharmaceutical
production, and fermentation of various products.
There are some advantages and disadvantages of using batch reactor in chemical reaction. The
advantages of the batch reactor lie with its versatility. A single vessel can carry out a sequence of
different operations without the need to break containment. This is particularly useful when
processing toxic or highly potent compounds. Since the reactor can be operated in batches, it can
be used as a viable model that can be applied for the biological treatment of wastewater released
by industries.

The batch wise operation also makes it possible to handle the industrial wastewater that can vary
significantly in its characteristics and in its volume from time to time. The disadvantages of batch
reactor include, inherent down-time between batches, unsteady-state operation means process
control and obtaining uniformity of product is more difficult and process control and obtaining
uniform product quality more difficult because of unsteady-state operation. It is also a high
operating cost and the product quality more variable than with continuous operation.
 2. Write a one-paragraph summary of any journal article that studies chemical
reaction in a batch reactor. The article must have been published within the last 5
years. Explain on the batch reactor used in the study and its significance to the
study done.

The reaction of polyol and isocyanate monomers to form polyurethanes is commonly presented in
reaction chemistry that implies a step-growth mechanism for the polymerization. However,
viscosity versus temperature profiles of both experimental studies and gel-forming simulation
studies indicate that the degree of polymerization resulting from the reactions varies considerably
from reactions with catalysts compared with those without catalysts. An extension of a simulation
based solely on step-growth mechanisms to simulations that include chain growth via an active
catalytic complex provides viscosity and temperature profiles that are consistent with the range of
experimental data. The results indicate that as catalytic mechanisms dominate the kinetics chain
growth mechanisms also overwhelm step growth mechanisms. Based on this mechanism, the
choice of catalysts can impact both the rate of reaction and degree of polymerization length; both
being of high importance in engineering urethane foams.

.
APPENDICES
Table 4: The value of Conductivity (mS/cm) and Concentration of NaOH (M).

Conductivity (mS/cm) Concentration of NaOH (M)

4 0

5.6 0.0125

7.5 0.025

9.7 0.0375

10.7 0.05

CALCULATION
Determine the rate constant, k, from the slope of graph 1/CA vs time,t.
1/CA = kt + 1/CAO
0
(At 40 C)
y = 1.1412x + 30.005
K = 1.1412
ln K = 0.1321

(At 500C)
y = 0.51x + 41.106
K = 0.51
ln K = -0.6931

The equation from the graph is;

y = -0.825x + 0.9573
Therefore,
ln k = ln A – Ea
RT
ln k = ln 0.9573 – 0.825 ( Equation 1)

The slope is -0.825 and the y-axis intercept which is frequency factor, A, are 0.9573.
i. The activation energy, Ea at 40º C

ln k = ln A - Ea
RT
Ea = RT (ln A – ln k)
Ea = (8.3014 J/mol.k × 313.15k) × (ln 0.9573 – ln 1.1412)

Ea = -0.1136 KJ/mol

ii. B. The activation energy, Ea at 50º C

ln k = ln A - Ea
RT
Ea = RT (ln A – ln k)
Ea = (8.3014 J/mol.k × 323.15k) × (ln 0.95873 – ln 0.51)

Ea = -0.1164 KJ/mol