Mutah University

Faculty of Engineering
Department of Chemical Engineering

Reaction Engineering Lab 0404422

A Report About Measurement Batch Reactor (Integral Method)

Experiment no. 2

Instructors: Dr. Alanood A. Al Sarayreh

Eng. Assia Al Garalleh

Student Name Student Number

Rayan Othman Al Masri 120210414078
Arwa Musallam Lassassmeh 120210414019
• Abstract
This experiment aimed to determine the reaction order and rate constant for the
saponification of ethyl acetate with sodium hydroxide using a batch reactor. The
integral method was employed by analysing conductivity data collected over
time, serving as an indirect measure of hydroxide ion concentration. Various
kinetic models were tested, and the second-order rate law provided the best fit.
The experimentally determined rate constant was kexp=0.2058 L\mol∙s, while the
theoretical value is ktheoretical=0.111 L\mol∙s, yielding a percentage error of
85.41%. The deviation is attributed to instrumental limitations, mixing
inconsistencies, and environmental factors.
• Introduction

In chemical reaction engineering, kinetic studies are essential for understanding

reaction mechanisms and for designing reactors. Batch reactors are ideal for
such investigations, as they allow for precise control over reactant
concentrations and reaction conditions. The saponification of ethyl acetate by
sodium hydroxide is a well-characterized reaction with a 1:1 stoichiometric
ratio and is often used to model second-order kinetics.

This experiment focuses on determining the overall order and rate constant of
the saponification reaction using the integral method. By measuring the
conductivity of the solution over time, which reflects the decreasing
concentration of hydroxide ions, different kinetic models are evaluated to
identify the best fit. The experimentally obtained rate constant is then compared
to the known theoretical value to assess accuracy and potential sources of error.

• Objectives
1. To identify the overall order of the saponification reaction based on
experimental kinetic data.
2. To determine the reaction rate constant for the saponification reaction of
ethyl acetate under controlled conditions and compare it to the
theoretical value.
3. To investigate the performance and operational characteristics of a batch
reactor system.
• Theory
A batch reactor is a closed system in which all reactants are introduced at the
beginning and no materials are added or withdrawn during the reaction. Batch
reactors are widely used in:
- Small-scale or laboratory-scale production,
- Testing and developing new chemical processes,
- Manufacturing of high-value products,
- Reactions unsuitable for continuous operation due to safety or control
challenges.

This reactor type allows precise control over operating parameters such as
temperature, pressure, and reaction time, making it particularly suitable for
kinetic studies and experimental validation.
The reaction under study is the saponification of ethyl acetate by sodium
hydroxide:
CH3COOC2H5 + NaOH → CH3COONa + C2H5OH
In aqueous solution:
- Sodium hydroxide dissociates completely into (Na+ ) and hydroxide ions
(OH − )
- Ethyl acetate undergoes nucleophilic attack by (OH − )on the carbonyl
group.
- The reaction yields sodium acetate and ethanol.
This process is commonly used as a model reaction for kinetic studies due to its
relatively simple mechanism and clear stoichiometry.
The general rate law for a second-order reaction is:
−rA = kCA CB
Or in differential form:
dCA
−rA = = kCA CB
dt
Where:
- −rA : Rate of reaction with respect to species A (mol/L·s)
- k: Rate constant (its units depend on the order of the reaction
- CA : Concentration of NaOH (mol/L),
- CB : Concentration of CH3COOC2H5 (mol/L)

An overall second-order rate expression is initially assumed based on the

stoichiometry and established reaction mechanism. To validate this assumption,
the integral method of analysis is applied. This method involves testing
different integrated rate laws—such as first-order and second-order forms—
against experimental data. The correct reaction order is identified by
determining which linearized plot provides the best fit. This approach allows for
both confirmation of the reaction order and accurate determination of the rate
constant k.
From the stoichiometry of the reaction, the concentration of sodium hydroxide
at any conversion xxx is given by:
CA = CA0 (1 − x)
Where:
- CA0 : Initial concentration of reactant NaOH at time t=0.
- x : Conversion of reactant A
Assuming a pseudo-first-order condition or symmetrical second-order
conditions, the rate becomes:
−rA = kCA 2
Substituting equation (2) into (3) and integrating yields:
CA0 − CA
kt =
CA0 × CA
This expression allows the experimental determination of the rate constant k by
tracking changes in concentration over time.
Sodium hydroxide is a strong electrolyte, and its dissociation contributes
significantly to the solution’s conductivity. As the reaction proceeds and
hydroxide ions are consumed, a corresponding decrease in conductivity occurs.
Thus, electrical conductivity serves as a reliable indirect measure of reaction
progress.

The fractional conversion ( x) can be calculated from conductivity readings

using:
λ∞ − λ
x=1−
λ∞ − λ0
where:
- x is the fractional conversion,
- λ0 is the initial conductivity,
- λ is the conductivity at time t,
- λ∞ is the conductivity at complete reaction.

This expression can be written in terms of concentration:

CA λ − λ∞
=
CA0 λ0 − λ∞

This method assumes that conductivity changes are primarily due to the
depletion of (OH − ) ions and that the contribution of the products to
conductivity is relatively minor.
• Chemicals
- NaOH pellets
- Solid CH₃COONa
- Distilled Water

• Apparatus & Glassware

- Magnetic Stirring Bars
- Magnetic Stirrer Hotplate
- Conductivity Meter
- Volumetric Flasks
- Graduated Cylinders
- Beakers
- Batch Reactor (Experimental Setup)

Figure 1: Magnetic Bar Figure 2: Magnetic Stirrer Hotplate Figure 3: Conductivity Meter

Figure 4: Beaker Figure 5: Graduated Cylinder Figure 6: Volumetric Flask

Figure 8: Batch Reactor (Experimental Setup)

• Procedure
1. Preparation of 0.1 M Ethyl Acetate Solution (Stock)
- Measure 9.79 mL of ethyl acetate (density = 0.9 g/cm³; molar mass = -
88.11 g/mol) using a graduated pipette.
- Transfer the measured volume into a 1 L volumetric flask and dilute
with distilled water up to the 1000 mL mark.
- Seal the flask securely and shake vigorously to ensure complete
mixing.
2. Preparation of 0.1 M Sodium Hydroxide Solution (Stock)
- Weigh 4 g of sodium hydroxide pellets (molar mass = 40 g/mol) and
dissolve them in a 1 L volumetric flask.
- Add distilled water to bring the volume up to 1000 mL.
- Cap the flask and shake thoroughly until fully dissolved.
3. Preparation of 0.05 M Diluted Solutions
- Measure 250 mL of the 0.1 M ethyl acetate stock solution and dilute
with 250 mL of distilled water to prepare 500 mL of 0.05 M ethyl
acetate.
- Similarly, take 250 mL of the 0.1 M sodium hydroxide stock solution
and dilute with 250 mL of distilled water to prepare 500 mL of 0.05 M
sodium hydroxide.
- Mix both diluted solutions thoroughly before use.
4. Conducting the Reaction
- Transfer 250 mL of the 0.05 M sodium hydroxide solution into the
batch reactor.
- Allow the solution to reach thermal equilibrium.
- Set the stirrer to medium speed, but do not activate it yet.
- Add 250 mL of the 0.05 M ethyl acetate solution into the reactor.
- Start the stirrer and begin timing the reaction.
- Measure and record the conductivity and temperature at regular
intervals for approximately 30 minutes.

• Safety Precautions
1. Wear appropriate PPE when handling sodium hydroxide, including
gloves, lab coat, and eye protection, to prevent chemical burns and eye
injury.
2. Conduct all work with ethyl acetate in a fume hood to avoid inhalation
of flammable and irritating vapours.
• Data & Calculations
- Experimental Data

In this experiment, 250 mL of 0.05 M sodium hydroxide solution and 250

mL of 0.05 M ethyl acetate solution were used for the saponification
reaction. These volumes were mixed in a batch reactor, and data
collection was initiated immediately after stirring began at a temperature
of 23 °C.

Table 1: Experimental Data

Time (s) λ (mS/cm) CA (𝐌) 𝐥𝐧 𝐂𝐀 (𝐌) 𝟏⁄𝐂𝐀 (𝐌)
0 6.13 0.02500 -3.68888 40
5 6.08 0.02459 -3.70542 40.66
10 6.03 0.02418 -3.72223 41.35
15 5.88 0.02297 -3.77357 43.53
20 5.80 0.02232 -3.80227 44.8
25 5.73 0.02175 -3.82814 45.97
30 5.70 0.02150 -3.8397 46.51
35 5.63 0.02094 -3.86609 47.75
40 5.60 0.02069 -3.8781 48.33
45 5.55 0.02029 -3.89763 49.28
50 5.50 0.01988 -3.91804 50.30
55 5.45 0.01948 -3.93837 52.33
60 5.42 0.01923 -3.95128 52
∞ 3.05 -
Calculation Samples:
- To determine λ0 , extrapolation is used.
1. Calculate the slope using these points:
(5,6.08) (10,6.03)
6.03 − 6.08
slope = = −0.01
10 − 5

2. Find the line’s equation:

y − y1 = m (x − x1 )
y − 6.08 = −0.01 (x − 5)
y = −0.01x + 6.13
3. Find the value of λ0 at t=0:
y = −0.01(0) + 6.13 = 6.13 mS⁄cm

- To determine the initial concentration of NaOH:

CA 0.05 M
CA0 = = = 0.025 M
2 2

- To determine the concentration CA , use the following formula:

CA λ − λ∞
=
CA0 λ0 − λ∞

At t = 0, λ0 = 6.13, λ∞ = 3.05 and CA0 = 0.025 M

6.13 − 3.05
CA = × 0.025 = 0.025 M
6.13 − 3.05
- Assume the Overall Reaction Order
Since equimolar amounts of the reactants were used and the
stoichiometric ratio of the saponification reaction is 1:1, the
concentrations of sodium hydroxide and ethyl acetate remain equal
throughout the reaction, CA = CB .
As a result, the general rate law:

−rA = CA α CB β

−rA = CA α+β

This expression indicates that the overall reaction order is the sum of the
partial orders with respect to each reactant:
γ = α+β
−rA = CA γ
▪ Zero Order: γ = 0
−rA = k

dCA
− =k
dt

−dCA = k dt

CA t
∫ − dCA = ∫ k dt
CA0 0

CA = CA0 + kt
▪ First Order γ = 1
−rA = kCA

dCA
− = kCA
dt

− dCA
= k dt
CA

CA t
− dCA
∫ = ∫ k dt
CA0 CA 0

ln CA = ln CA0 − kt

▪ Second Order γ = 2
−rA = kCA

dCA
− = kCA 2
dt

− dCA
= k dt
CA 2

CA t
− dCA
∫ = ∫ k dt
CA0 CA 2 0

1 1
= + kt
CA CA0
• Results

TIME VS. 𝐶𝐴
7

4
CA ( M )

0
0 50 100 150 200 250 300
TIME (S)

Figure 8: Zero-order kinetic plot: Concentration of NaOH vs. time.

- This figure shows the relationship between the concentration of sodium

hydroxide and time.

TIME VS. 𝐶𝐴
0.03

0.025

0.02
CA ( M)

0.015
y = -1E-04x + 0.0247
R² = 0.9707
0.01

0.005

0
0 10 20 30 40 50 60 70
TIME (S)

Figure 9 First-order kinetic plot: ln (Concentration of NaOH) vs. time.

- This figure represents the plot of the natural logarithm of sodium

hydroxide concentration versus time. The deviation from linearity
suggests that the reaction does not follow first-order kinetics.
 LN CA VS. TIME
-3.65
0 10 20 30 40 50 60 70
-3.7

-3.75
y = -0.0045x - 3.6969
R² = 0.9806
LN CA ( M )

-3.8

-3.85

-3.9

-3.95

-4
TIME (S)

Figure 10 Second-order kinetic plot: 1 / Concentration of NaOH vs. time.

- This figure shows the plot of the reciprocal of sodium hydroxide

concentration versus time. The strong linearity supports the hypothesis
that the reaction follows second-order kinetics.

TIME VS. 1∕𝐶𝐴

60

50

40
y = 0.2058x + 40.12
1∕𝐶𝐴 ( M )

R² = 0.988
30

20

10

0
0 10 20 30 40 50 60 70
TIME (S)

Figure 11 Comparison of linear fits for zero, first, and second-order models.

- This figure compares the linear fits for zero, first, and second-order
models. The second-order plot shows the best linear fit with the highest
R² value.
▪ From the graphical analysis, the second-order kinetic model provided the
best linear fit, yielding an experimental rate constant k=0.2058 L \mol∙s.
• Discussion
The experiment demonstrated that the saponification of ethyl acetate with
sodium hydroxide follows second-order kinetics. This conclusion is supported
by the high linearity observed in the second-order kinetic plot of 1/[CA] versus
time. The integral method effectively confirmed the reaction order, consistent
with the known 1:1 stoichiometry and equimolar initial concentrations of the
reactants.
The experimentally determined rate constant was:
kexp=0.2058 L\mol∙s
This value was compared to the theoretical rate constant:
ktheoretical=0.111 L\mol∙s
The percentage error was calculated using:
experimental value − theoritical value
ϵ%= | | × 100%
theoritical value

0.2058 − 0.111
ϵ%= | | × 100% = 85.40%
0.111

This notable deviation suggests the presence of several potential sources of

error, including:
- Instrumental inaccuracies in the conductivity meter,
- Delay in starting the timer precisely now of mixing,
- Temperature fluctuations, as the reaction rate is temperature-sensitive,
- Incomplete or inconsistent mixing, particularly at the early stages of the
reaction,
- Human error in handling measurements or solution preparations.
Despite this error, the shape of the kinetic plots and the relative trends clearly
support second-order behaviour. The integral method, combined with
conductivity measurements, proved effective for kinetic evaluation in a batch
reactor.
• Conclusion
This experiment successfully confirmed that the saponification reaction between
ethyl acetate and sodium hydroxide follows second-order kinetics under
equimolar conditions in a batch reactor. The reaction rate constant was
determined experimentally to be k=0.2058 L\mol∙s, compared to the theoretical
value of 0.111 L\mol∙s. The calculated percentage error of 85.41% highlights the
impact of experimental limitations. Nonetheless, the findings support the
second-order nature of the reaction and demonstrate the effectiveness of using
conductivity data and the integral method in kinetic analysis.