1.

0 SUMMARY

The objectives of this experiment is to investigate the effect of temperature on

the saponification reaction between ethyl acetate (Et(Ac)) and sodium hydroxide
(NaOH). There were two different temperature used in this experiment which are 30℃
and 40℃. Firstly, before the experiment was started, the solution of sodium hydroxide
(NaOH) and ethyl actetate (Et(Ac)) were prepared separately and diluted with distilled
water. Then, both solutions were transferred into the reactor which the reactor used is
batch reactor. Next, the samples were drawn for every 5 minutes interval and
measured the conductivity by using conductivity meter. The process was repeated
until the result of conductivity is constant. Based on this experiment, the concentration
of sodium hydroxide decreased with the conductivity decreased for both temperature.
Besides, the conversion was also increased and slightly decreased as the time
increased for both temperature. Therefore, the conductivity is inversely proportional to
conversion. In addition, the rate of reaction was affected by temperature 40℃ has the
highest conversion compared to 30℃. Next, the 1/CA increased as the time also
increased for both temperature because when the time of the reaction longer, the
concentration of sodium hydroxide (NaOH) will decrease. The rate constant (k) were
determined which are 1.2116 for 30℃ and 3.5303 for 40℃. Lastly, the ln k is inversely
proportional to 1/T. In addition, the saponification reaction’s activation energy (E a)
obtained is 2.819 J/mol and the frequency factor is 1.1042 x 1014.
2.0 DATA AND RESULTS

Volume of NaOH : 3L
Volume of Et(Ac) : 3L
Temperature : 30 °C

Table 2.0: Effect of temperature on the batch saponification reaction at 30°C.

Time Temperature Conductivity Concentration of NaOH, Conversion,

(min) (°C) (mS/cm) CNaOH (M) X
*From Calibration Curve (%)
0 29.7 6.20 0.01625 0.00
5 30.0 6.00 0.01475 9.23
10 30.0 5.70 0.01250 23.08
15 30.0 5.50 0.01100 32.31
20 30.0 5.30 0.00975 40.00
25 30.0 5.30 0.00975 40.00
30 30.0 5.20 0.00900 44.62
35 30.0 5.20 0.00900 44.62
40 30.0 5.10 0.00800 50.77
45 30.0 5.10 0.00800 50.77
50 30.0 5.10 0.00800 50.77
55 30.0 5.10 0.00800 50.77
Volume of NaOH : 3L
Volume of Et(Ac) : 3L
Temperature : 40 °C

Table 2.1: Effect of temperature on the batch saponification reaction at 40°C.

Time Temperature Conductivity Concentration of NaOH, Conversion,

(min) (°C) (mS/cm) CNaOH (M) X
*From Calibration Curve (%)
0 40.00 5.60 0.01175 0.00
5 40.00 5.50 0.01100 6.38
10 40.00 5.20 0.00875 25.53
15 40.00 5.00 0.00725 38.30
20 40.00 4.80 0.00600 48.94
25 40.00 4.70 0.00500 57.45
30 40.00 4.70 0.00500 57.45
35 40.00 4.65 0.00450 61.70
40 40.00 4.65 0.00450 61.70
45 40.00 4.65 0.00450 61.70
 70

60

50
Conversion, X (%)

40

30℃
30
40℃
20

10

0
0 10 20 30 40 50 60
Time (min)

Figure 2.0: A graph of conversion, X (%) against time (min) for both temperature.
 Table 2.1: Data calculated for both temperature.

Temperature: 30℃ Temperature: 40℃

Time Concentration of Concentration of NaOH,

(min) NaOH, CNaOH (M) 1/CA CNaOH (M) 1/CA
*From Calibration Curve *From Calibration Curve
0 0.01625 0.01175
61.54 85.11
5 0.01475 0.01100
67.80 90.91
10 0.01250 0.00875
80.00 114.29
15 0.01100 0.00725
90.91 137.93
20 0.00975 0.00600
102.56 166.67
25 0.00975 0.00500
102.56 200.00
30 0.00900 0.00500
111.11 200.00
35 0.00900 0.00450
111.11 222.22
40 0.00800 0.00450
125.00 222.22
45 0.00800 0.00450
125.00 222.22
50 0.00800
125.00
55 0.00800
125.00
 160.00

140.00 y = 1.2116x + 68.981

120.00

100.00
1/CA

80.00
30℃
60.00
Linear (30℃)
40.00

20.00

0.00
0 10 20 30 40 50 60
Time (min)

Figure 2.1: A graph of 1/CA against time at 30℃ and the slope obtained is 1.2116.

Rate constant, k for 30℃ is 1.2116. 40℃ is 3.5303

300.00

250.00 y = 3.5303x + 86.726

200.00
1/CA

150.00
40℃

100.00 Linear (40℃)

50.00

0.00
0 10 20 30 40 50
Time (min)

Figure 2.2: A graph of 1/CA against time at 40℃ and the slope obtained is 3.5303.

Rate constant, k for 40℃ is 3.5303.

 1.4

1.2
y = -9722.7x + 32.277
1

0.8
ln k

0.6

0.4

0.2

0
0.00318 0.0032 0.00322 0.00324 0.00326 0.00328 0.0033 0.00332
1/T (K-1)

Figure 2.3: A graph of ln k against 1/T and the slope obtained is -9722.7.

From the graph plotted:

Ea = 2.819 J/mol

A = 1.1042 x 1014
3.0 ANALYSIS AND DISCUSSION

The objectives of this experiment is to examine the effect of temperature on the

reaction between ethyl acetate (Et(Ac)) and sodium hydroxide (NaOH). This reaction is
called as saponification reaction and it was done under batch reactor. Saponification is a
process where the oil or fat was mixed with a strong base or alkali to produce soap and
glycerin. Batch reactor is one of the reactor that extensively used in process industries
and it is a reactor where the steady state process developed. In addition, batch reactor is
the placed for the reaction to continue at given time which the unreacted reactants and
product is withdrawn simultaneously. The saponification reaction in this experiment can
be expressed by the stoichiometric equation below:

In this experiment, there were two distinct temperature used which are 30℃ and
40℃. For both temperature, the conductivity of all samples that withdrawn for every 5
minutes was delibrated and the concentration of sodium hydroxide (NaOH) and
conversion were calculated. Hence, based on Table 2.0 and 2.1, the concentration of
sodium hydroxide was determined by the calibration curve, as shown in Appendix A.
Based on the data tabulated on Table 2.0 and 2.1, concentration of sodium hydroxide
decreased with the conductivity decreased.

From Figure 2.0, the conversion increased and slightly decreased as the time
increased for both temperature but the highest conversion obtained at 40℃ compared to
30℃. This result can be supported by the theory, the conductivity increased as the
conversion decreased. Thus, conductivity is inversely proportional to conversion. In
addition, the rate of reaction will affected by temperature which this can be interpreted by
the result obtained, higher temperature has higher conversion. This also can be
supported by the theory which when the temperature increased, the movement of the
particles vibrate increasingly and this affected the particles to collide to each other.
Therefore, it will cause the reaction increase because the movement particles increase
and release the energy.

Next, a graph of 1/CA against time for both temperature were plotted because the
reaction follows the second order reaction. Based on Figure 2.1 and 2.2, both temperature
have same pattern which 1/CA increased as the time increased. This can be explained as
the time of the reaction is longer, the concentration of sodium hydroxide (NaOH) will
decrease and reduced to form the product. Besides, in this experiment, sodium hydroxide
was the limiting reactant. Thus, when the concentration of sodium hydroxide is inversely,
it will become increased. Based on the graphs plotted, the rate constant (k) were
determined which are 1.2116 for 30℃ and 3.5303 for 40℃. Lastly, a graph of ln k against
1/T was plotted to evaluate the saponification reaction’s activation energy (E a) and the
frequency factor (A). Based on Figure 2.3, the ln k is inversely proportional to 1/T.
Therefore, based on this result obtained, it can support that this saponification reaction is
a second order reaction. In addition, the saponification reaction’s activation energy (E a)
obtained is 2.819 J/mol and the frequency factor is 1.1042 x 1014.
4.0 CONCLUSION AND RECOMMENDATIONS

4.1 CONCLUSIONS

The objectives of this experiment is to investigate the effect of temperature on the

saponification reaction between ethyl acetate (Et(Ac)) and sodium hydroxide (NaOH).
There were two different temperature used in this experiment which are 30℃ and 40℃.
For both temperature, the concentration of sodium hydroxide decreased with the
conductivity decreased. In addition, the conversion increased and slightly decreased as
the time increased for both temperature. Thus, conductivity is inversely proportional to
conversion. The rate of reaction was affected by temperature because a higher
temperature has higher conversion which 40℃ has the highest conversion compared to
30℃. Next, when the 1/CA increased, the time also increased for both temperature
because as the time of the reaction is longer, the concentration of sodium hydroxide
(NaOH) will decrease as sodium hydroxide was the limiting reactant. Thus, when the
concentration of sodium hydroxide is inversely, it will become increased. The rate
constant (k) were determined which are 1.2116 for 30℃ and 3.5303 for 40℃. Lastly, the
ln k is inversely proportional to 1/T. because this saponification reaction is a second order
reaction. In addition, the saponification reaction’s activation energy (Ea) obtained is 2.819
J/mol and the frequency factor is 1.1042 x 1014.
4.2 RECOMMENDATIONS

There are a few steps that can be taken to prevent the errors which firstly, before
the experiment was started, all team members need to examine the manual of to prevent
misleading process. All the valves need to double check if it is open or closed according
to the manual. Next, this experiment is a time consuming because the process need to
heat and cool down the reactor according to the desired temperature set up. The reactor
temperature must be same with the desired temperature to avoid any error that might
affected the results. Besides, as the readings of the conductivity remain constant, the
process can be stopped. There must be a few possible errors occurred during carry out
the conductivity meter and this might be affected the results. This errors can be possibly
occurred because of the conductivity meter’s rod is not clean and the rod must be wiped
before measured other samples.
5.0 TUTORIAL

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

utilized batch reactors in its process.

Biopharmaceutical production is one of the example that utilized batch reactors

in its content. Batch reactors are jacketed vessels that come in a variety of sizes,
and mostly used to synthesize pharmaceutical ingredients. By application batch
reactor it is produce benzoic acid that used in our daily application such as used
chemical ingredient in the production of food as antimicrobial additive, converting
caprolactam which is monomer used in industrial production of nylon fibers, it also
utilized in medicine and cosmetic products. The reaction is about to synthesis the
ethylbenzoate with ethanol, water and sodium hydroxide in batch reactor at 40̊ C at
optimum temperature (Gleason & Shah., 2013). Hence, the making benzoic acid
from ethyl benzoate is a model reaction that shows how some pharmaceutical
ingredients are made using a batch reactor.

The advantages and disadvantages of using batch reactors in chemical

reaction:
Advantages Disadvantages

 High conversion per unit volume for  High operating cost

pass
 Difficult to control exothermic reaction
 Easier to cater for slow reaction
 Risk of contamination if more than one
 Same vessel used ( no flow in/out product made in reaction vessel.
at the same time)
 Product quality more variable than with
 Easy to clean continuous operation
2. Summarize 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 significant to the study done.

The article titled “An Analysis of Adiabatic Batch Reactor” written by Arcadii,
Scott, and Laura. During this research, an adiabatic batch reactor is to be said, is
relevant to fields pertaining to the prediction of temperature in chemical reactions; in
determining the temperature reached and concentration of reactants left. Besides,
this reactor is precisely used in a small scale laboratory applications, for example,
the production and introduction of fermentation of beverage products. Batch reactors
are also importantly used in the field of waste water treatment due to their
effectiveness in decreasing the biological oxygen demand (BOD) of waste water
(Asiedu et al, 2013). The goal of this study from an adiabatic batch reactor is to
determine the temperature, concentration of a mixture and time needed for the
hydrolysis of acetic anhydrate mixture that is reacted with excess water in the reactor
to form an exothermic reaction. An adiabatic reactor is insulated on order to prevent
any heat exchange with its surroundings. Reaction progress was tracked by actual-
time under various temperature of conditions. The variables examined for
comparative study are concentration, Due to the Fritzer et al (2014), heat will be
released and the temperature inside the adiabatic reactor will increased since the
reaction is exothermic, hence, the highest temperatures will cause the reaction to
occur faster. The rate reaction increases with increase of temperature in case of
batch reactor under studies range of temperature. The results obtained in this
investigation may be useful in maximing the industrial level of production of desired
product. Hence, in the future projects would be easier resolve the chemical reaction
that provide more accurate results after a certain amount of time. The advantages
of batch reactor include the low difficulty to cater for slow reactions and capability of
high conversion per unit volume for pass.
6.0 REFERENCES

Ahmad., A., Imran., M. A., Younas., M., Khan., H., & Shah., M. H. (2013). A comparative
study of alkaline hydrolysis of ethyl acetate using design of experiments. Iranian
Journal of Chemistry and Chemical Engineering. 32(4): 33 – 47.

Ahmed., A. M. A. (2010). Saponification: A comparative kinetic study in a batch reactor.

Thesis of University of Khartoum in Chemical Engineering.

Arcadii., G., Scott., C., & Laura., A. (2013) An analysis of adiabatic batch reactor.
Undergraduate Journal of Mathematical Modelling. 12(6): Article 4

Asidue., Hilderbrandt., et al. (2013). Kinetic modelling of acetic anhydride at higher

temperatures using adiabatic batch reactor. Journal of Chemical Engineering &
Process Technology. 9(2013): 2 – 5.

Bursali., N., Ertunc., S. & Akay. (2006). Process improvement approach to saponification
reaction using statistical experimental design. Chemical Engineering Process. 45: 980
– 989.

Das., K., Sahoo., P., Baba., M. S., Murali., N., & Swainathan., P. (2011). Kinetic studies
on saponification of ethyl acetate using an innovative conductivity-monitoring
instrument with a pulsating sensor. International Journal of Chemical Kinetics. 43(11):
648 – 656.
Fritzer., B. C., et al. (2014). Acetic anhydride hydrolysis at high acetic anhydride to water
ratios. International Journal of Chemical Kinetics 46(2014): 151 – 160.

Gleason., P., P., & Shah., N., D. (2013). Patenting in the biopharmaceutical industry.
Journal of Nature Biotechnology 2.1(2013): 130 - 140

Mesfer., M. K. A. (2017). Experimental study of batch reactor performance for ethyl

acetate saponification. International Journal of Chemical Reactor Engineering. 16(1):
174 – 178.
7.0 APPENDICES

7.1 APPENDIX A

Calibration Curve:
7.2 APPENDIX B

Calculation for conversion, X (%):

A) Temp: 30°C

𝑪𝑁𝑎𝑂𝐻 (𝑡=0)− 𝑪𝑁𝑎𝑂𝐻 (𝑡) 𝑪𝑁𝑎𝑂𝐻 (𝑡=0)− 𝑪𝑁𝑎𝑂𝐻 (𝑡)

X= x 100% X= x 100%
𝑪𝑁𝑎𝑂𝐻 (𝑡=0) 𝑪𝑁𝑎𝑂𝐻 (𝑡=0)

0.01625 − 0.01475 0.01625 − 0.00800

= x 100% = x 100%
0.01625 0.01625

= 9.23 % = 50.77 %

B) Temp: 40°C

𝑪𝑁𝑎𝑂𝐻 (𝑡=0)− 𝑪𝑁𝑎𝑂𝐻 (𝑡) 𝑪𝑁𝑎𝑂𝐻 (𝑡=0)− 𝑪𝑁𝑎𝑂𝐻 (𝑡)

X= x 100% X= x 100%
𝑪𝑁𝑎𝑂𝐻 (𝑡=0) 𝑪𝑁𝑎𝑂𝐻 (𝑡=0)

0.01175 − 0.01100 0.01175 − 0.00450

= x 100% = x 100%
0.01175 0.01175

= 6.38 % = 61.70 %
7.3 APPENDIX C

Calculating rate constant:

For a second order reaction, the rate law is:

1 1
= 𝑘𝑡 +
𝐶𝐴 𝐶𝐴𝑂

Where k is rate constant, therefore the rate constant can obtained from the graph plotted
which are 1.2116 for 30℃ and 3.5303 for 40℃.

Calculating activation energy and frequency:

From the Arrhenius equation in linear form:

𝑘2 − 𝐸𝑎 1 1
𝑙𝑛 = ( − )
𝑘1 𝑅 𝑇1 𝑇2

0.00319 − 𝐸𝑎 1 1
𝑙𝑛 = ( − )
0.00330 𝐽 303.15 𝐾 313.15 𝐾
8.314
𝑚𝑜𝑙. 𝐾
𝐽
− 𝐸𝑎 = −2.819
𝑚𝑜𝑙
𝐽
− 𝐸𝑎 = 2.819
𝑚𝑜𝑙

ln A = 32.277
A = e(32.277)
A = 1.1042 x 1014