BIRLA INSTITUTE OF TECHNOLOGY AND SCIENCE, PILANI

Department of Chemical Engineering

First Semester 2023-2024

CHE F312 Chemical Engineering Laboratory-1
Laboratory Report

Name of TA and Signature:

Submission Date: 01/04/2024

Group Number: 10

Name ID

Palash Gagrani 2021A1PS2580P

A. Sai Puviiyarasu 2021A1PS2594P

Shubh Nema 2021A1PS2602P

Ayyappan Pillai 2021A1PS2370P

Experiment No: 1
Experiment Name: Isothermal Batch Reactor

1) Aim: To determine the reaction rate constant (k) for the given saponification
reaction of ethyl acetate in aqueous sodium hydroxide solution.

2) Objectives of the experiment:

● Study of a non-catalytic homogeneous reaction in a batch reactor.

3) Laboratory Observations:

● 9.8mL of Ethyl Acetate Added in 10 Litres Water to prepare N/10

Solution.
● 4g NaOH added in 10 Litres Water to prepare N/10 Solution.
● CA0=0.1N

Page 1 of 15
 At 60°C,

S. No. Time (min) Volume of sample Volume of Sample taken Volume of

taken (ml) N/10 HCl for titration N/10 NaOH
added to (ml) used for
sample (ml) titration (ml)

1 5 10 10 20 6.2

2 10 10 10 20 7.9

3 15 10 10 20 8.4

4 20 10 10 20 9.3

At 70°C,

S. No. Time (min) Volume of sample Volume of Sample taken Volume of

taken (ml) N/10 HCl for titration N/10 NaOH
added to (ml) used for
sample (ml) titration (ml)

1 5 10 10 20 7.2

2 10 10 10 20 8.1

3 15 10 10 20 8.4

4 20 10 10 20 8.9

Page 2 of 15
4) Sample Calculations:

For T = 60 ℃
At t = 10 min
For observation 2,
Vol. of N/10 HCl taken in flask = 10 mL
Vol. of sample taken = 10 mL
Vol. of N/10 NaOH used for titration = VNaOH
1
No. of moles of NaOH used = VNaOH * 10
* 10-3 gmol = 10-4 g.mol
1
No. of moles of HCl present initially in flask= 10 * 10 * 10-3 g.mol

= 10-3 g.mol

No. of moles of NaOH left in the sample = (10-3- VNaOH*10-4 )

−3 −4
(10 )− (𝑉𝑁𝑎𝑂𝐻 * 10 )
CA= −2 g.mol/L
10

−3 −4
(10 )− (7.2 * 10 )
VNaOH= 7.2 ml, CA = −2 g.mol/L
10

= 0.032 g.mol/L

For 1st order reaction,

-rA = k * CA

𝑑𝐶𝐴
Also, -rA = - 𝑑𝑡

𝑑𝐶𝐴
- 𝑑𝑡 = k * CA

Integration yields:

ln(CA) = ln(CA0) - (k * t)

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 For 2nd order reaction,

-rA = k * CA2

𝑑𝐶𝐴
Also, -rA = - 𝑑𝑡

𝑑𝐶𝐴
- 𝑑𝑡 = k * CA2

Integration yields:

1 1
𝐶𝐴
= (k * t) + ( 𝐶 )
𝐴0

5) Results and Discussion:

At 60℃,

t (min) C (g.mol/L) -ln(CA/CA0)

A
1/CA (L/g.mol)

5 0.038 0.967584026 26.31578947

10 0.032 1.139434283 31.25

15 0.029 1.237874356 34.48275862

20 0.02675 1.318635713 37.38317757

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Page 5 of 15
At 70℃,

t(min) CA(g.mol/L) -ln(CA/CA0) 1/CA(L/g.mol)

5 0.028 1.272965676 35.71428571

10 0.018 1.714798428 55.55555556

15 0.013 2.040220829 76.92307692

20 0.011 2.207274913 90.90909091

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 𝐸𝐴
k = A * exp(− 𝑅*𝑇
)

where,

A = Arrhenius constant

Ea = Activation energy

𝐽
R = ideal gas constant = 8.314 𝑔.𝑚𝑜𝑙 − 𝐾

This equation can be written as,

𝐸 1
ln(k) = − 𝑅
( 𝑇 ) + ln(k0)

Thus, (E/R) can be calculated from the graph of ln K vs 1/T:

k lnk T 1/T

0.7287 -0.316493154 333.15 0.003001651

Page 7 of 15
3.739 1.318818196 343.15 0.002914177

We get,

𝐸
Slope = − 𝑅
= -18695

E = -(-18695) * 8.314

𝐽
= 155430.23 𝑔.𝑚𝑜𝑙

Page 8 of 15
 The below table shows the concentration of NaOH left in the sample for the 2
different temperatures.

Reaction Temperature = 60 °C

Time Concentration of
(min) NaOH

left in the sample

5 0.038

10 0.032

15 0.029

20 0.02675

Reaction Temperature = 70 °C

Time Concentration of
(min) NaOH

left in the sample

5 0.028

10 0.018

Page 9 of 15
15 0.013

20 0.011

As shown in the sample calculations, 2 models, one for a first-order reaction and the
other for a second-order reaction are fitted to the experimental data.

The plot for the second-order reaction appears to be a marginally better fit than that
for the first-order reaction. This can be observed by the R2 value for the 2 plots. The

second-order reaction fit has an R2 value of 0.9929 while that of the first-order

reaction fit has an R2 value of 0.9627.

Based on this, we can conclude that the saponification reaction is following 2nd
order rate kinetics based on whatever data was experimentally available.

Using the 2nd order rate kinetics equation, the value of the rate constant for the 2
reaction temperatures was found out as follows:

Reaction Reaction
Constant (k) Temperature

0.7287 60 °C

3.739 70 °C

The above table has an agreeable relation with the theoretical expectations which
suggest that as the temperature at which the reaction is carried out increases, the
rate constant would also increase.

Page 10 of 15
 The activation energy of the reaction is found to be 155430.23 J/g.mol

A Sai Puviiyarasu:
● The experimental data was analyzed using two models: one for a first-order
reaction(Graphs 1 and 3) and another for a second-order reaction (Graphs 2 and
4).
● The fit for the second-order reaction appears slightly superior, indicated by its
higher R2 value (0.9833) compared to the first-order reaction fit (R2 = 0.9675)
for 60℃.
● This suggests that the saponification reaction likely follows second-order
kinetics based on the available experimental data. Subsequently, the rate
constant values for the two reaction temperatures were determined using the
second-order kinetics equation.

Palash Gagrani:
● The experimental data was analyzed using two models: one for a first-order
reaction(Graphs 1 and 3) and another for a second-order reaction (Graphs 2 and
4).
● The fit for the second-order reaction appears slightly superior, indicated by its
higher R2 value (0.9833) compared to the first-order reaction fit (R2 = 0.9675)
for 60℃.
● This suggests that the saponification reaction likely follows second-order
kinetics based on the available experimental data. Subsequently, the rate
constant values for the two reaction temperatures were determined using the
second-order kinetics equation.
● The comparison of the rate constants obtained from the second-order kinetics
equation for different temperatures indicates that the reaction rate increases
with temperature. This is consistent with the expected behavior for chemical
reactions, where higher temperatures typically result in faster reaction rates due
to increased molecular collisions.
● The Arrhenius equation can be applied to further understand the temperature
dependence of the reaction rate constants. By plotting the natural logarithm of
the rate constants against the reciprocal of the absolute temperature (in Kelvin),
it's possible to determine the activation energy of the reaction. This analysis
provides insights into the energy barrier that molecules must overcome for the
reaction to occur.

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● The excellent fit of the second-order kinetics model to the experimental data
suggests that the assumptions underlying this model are appropriate for
describing the saponification reaction under the given conditions. However, it's
essential to consider potential limitations and assumptions of the model, such
as the absence of side reactions or variations in reactant concentrations.

Shubh Nema:
● Two models were used to assess the experimental data: Graphs 1 and 3
were used for a first-order reaction, while Graphs 2 and 4 were used for
a second-order reaction.
● Compared to the first-order reaction fit (R2 = 0.9675) for 60°C, the
second-order reaction fit looks to be slightly better, as seen by its
higher R2 value (0.9833).
● Based on the available experimental data, this indicates that the
saponification reaction most likely follows second-order kinetics. The
second-order kinetics equation was then used to get the rate constant
values for the two reaction temperatures.

Ayyappan Pillai:
● The experimental data was evaluated using two models: Graphs 1 and 3 were
utilized to analyze a first-order reaction, while Graphs 2 and 4 were utilized to
analyze a second-order reaction.
● The second-order reaction fit appears to be somewhat better than the
first-order reaction fit (R2 = 0.9675) for 60°C, as shown by its higher R2 value
(0.9833).
● This suggests that the saponification reaction most likely follows second-order
kinetics based on the existing experimental data. The rate constant values for
the two reaction temperatures were then obtained using the second-order
kinetics equation.

6) Conclusion:

A Sai Puviiyarasu:
● The reaction rate constant (k) increases with temperature. This is evident from
the higher k value at 70°C (3.739) compared to 60°C (0.7287).

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● The presence of a high activation energy suggests that the saponification
reaction may involve a complex mechanism with multiple steps or
intermediates.
● It also indicates strong interactions between ethyl acetate, water, and hydroxide
ions.
● The observed activation energy signifies the temperature sensitivity of the
saponification reaction. Careful control of reaction temperature is essential for
achieving desired reaction rates and product yields.

Palash Gagrani:
● Temperature causes an increase in the response rate constant (k). The fact that
the k value is larger at 70°C (3.739) than it is at 60°C (0.7287) indicates this.
● The saponification process may entail a complicated mechanism with several
stages or intermediates, as suggested by the high activation energy.
● Additionally, it shows that ethyl acetate, water, and hydroxide ions interact
strongly.
● The saponification reaction's temperature sensitivity is indicated by the
measured activation energy. To achieve the appropriate reaction rates and
product yields, careful reaction temperature control is necessary.
● The high activation energy associated with the saponification reaction suggests
a complex reaction mechanism involving multiple steps or intermediates.
● This complexity may arise from the involvement of various species, such as
ethyl acetate, water, and hydroxide ions, and their interactions during the
reaction process. Understanding the intricacies of the reaction mechanism is
crucial for developing effective strategies to control and optimize the reaction
conditions.
● The measured activation energy provides valuable information about the
energy barrier that must be overcome for the saponification reaction to proceed.
● The temperature sensitivity indicated by the activation energy underscores the
critical role of temperature control in modulating reaction kinetics and
achieving desired product outcomes. Optimal reaction temperatures can be
determined based on the activation energy to maximize reaction efficiency and
product yield.

Page 13 of 15
 Shubh Nema:
● Temperature causes an increase in the response rate constant (k). The
fact that the k value is larger at 70°C (3.739) than it is at 60°C (0.7287)
indicates this.
● The saponification process may entail a complicated mechanism with
several stages or intermediates, as suggested by the high activation
energy.
● Additionally, it shows that ethyl acetate, water, and hydroxide ions
interact strongly.
● The saponification reaction's temperature sensitivity is indicated by the
measured activation energy. To achieve the appropriate reaction rates
and product yields, careful reaction temperature control is necessary.
Ayyappan Pillai:
● The reaction rate constant (k) rises with temperature. This is
demonstrated by the fact that the k value is higher at 70°C (3.739) than
it is at 60°C (0.7287).
● The high activation energy suggests that the saponification process may
include a complex mechanism with several stages or intermediates.
● It also demonstrates the strong interaction between hydroxide ions,
water, and ethyl acetate.
● The observed activation energy provides information on the temperature
sensitivity of the saponification reaction. Careful reaction temperature
management is required to get the right reaction rates and product
yields.

7) References:

● Fogler H.Scott (2008). Elements of Chemical Reaction Engineering. 4th Ed.

Pearson Education, New Delhi, India.
● Levenspiel,”Chemical Reaction Engineering,” 2nd edition, John Wiley & Sons,
Singapore, 1995.
● Laboratory Manual for Chemical Engineering Laboratory– II by the
Department of Chemical Engineering, BITS Pilani.

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