Module 1: BKF3741 Chemical Reaction Engineering Laboratory

1.0 Title of Experiment

Saponification reaction of sodium hydroxide and ethyl acetate in a batch reactor Determination of
kinetic parameters using batch reactor

2.0 Objective
(a) To study the effects of temperature on saponification reaction of ethyl acetate and sodium
hydroxide in batch reactor.
(b) To determine the kinetic parameters and activation energy

3.0 Background
A batch reactor is used in chemical processes for small scale operation, for testing new processes
that have not been fully developed, for the manufacture of expensive products, and for processes that are
difficult to convert into continuous operations. The main advantage of a batch reactor is high conversion,
which can be obtained by leaving the reactant in the reactor for long periods of time, but it also has the
disadvantages of high labor costs per batch and the difficulty of large scale production. A batch reactor
can be used to find the reaction rate constant, activation energy and order of the reaction. The reaction
selected in this experiment is the liquid phase saponification reaction between sodium hydroxide (NaOH)
and EtOAc (ethyl acetate). This reaction is elementary and second-order. The reaction equation is

NaOH + EtOAc → NaOAc + EtOH

__________________________________________________________________________________
FKKSA/BKF3741/Module/Rev03/24/02/14
Module 1: BKF3741 Chemical Reaction Engineering Laboratory I

4.0 Apparatus
The apparatus as shown in Figure 1 is the batch reactor which is designed to study the kinetics of a
chemical reaction. It can conveniently be used to study the effects of varying the process conditions such
as reaction temperature, reactor volume and stirring rate on the reaction kinetics.

Figure 1 Experimental Setup

__________________________________________________________________________________
FKKSA/BKF3741/Module/Rev03092014
Module 1: BKF3741 Chemical Reaction Engineering Laboratory I

5.0 General Procedure

(i) The minimum working volume is 2 liter.
(ii) The conductivity of the reacting solution in the reactor changes with the degree of conversion and
this provides a convenient method for monitoring the progress of the reaction.
(iii) In this experiment, the conductivity can be recorded manually at suitable time intervals (hint:
every 2 minutes for the first 20 minutes and every 5 minutes for the subsequent reaction time) by
reading the value directly from the conductivity meter. The experiment should stop when the
reaction reaches steady state.
(iv) The reaction temperature can be varied (30-50 C) and maintained using the thermostat available
in accordance with the instructions given in the operating manual which is available near the
apparatus. You may choose any 2 temperatures for these experimental studies.

6.0 Conductivity Meter

The measurements of conductivity Λ are related to the conductivity of the NaOH and NaOAc
solution as follows:

Λ = ΛNaOH + ΛNaOAc

A series of mixtures with different proportion of 0.1 M sodium hydroxide (NaOH) solution and
0.1 M sodium acetate (NaOAc) solution could aid you in preparing a calibration curve to relate the
reaction conversion with the corresponding conductivity value.

__________________________________________________________________________________
FKKSA/BKF3741/Module/Rev03092014
Module 1: BKF3741 Chemical Reaction Engineering Laboratory I

7.0 Tasks and Questions

(i) Answers to the question should be submitted at the first 30 minutes of the class for that week.
Failure to submit answers in a timely fashion would affect the 50% of the total marks for the answers and
sample calculation part of the grade for the report.
(ii) The output of the tasks performed should be shown to the facilitator in the last hour of the class
for that week to ensure it has been done correctly.

7.1 Week 1
7.1.1 Questions
(i) Describe how do you find order of a reactant using differential/integral method of analysis? Give
the graph that would be used to prove that the reaction is first order with respect to both NaOH
and EtOAc.
(ii) What are the weights of NaOH, NaOAc and EtOAc to be added to 1 liter solution to obtain 0.1 M
solutions respectively? Calculate the weight required based on the purities and properties of the
chemicals provided in the laboratory.

7.1.2 Tasks
(i) Please read the reactor manual for general operation and safety.
(ii) List all the steps involved in details to generate the calibration curve based on the information
given in section 6.0.
(iii) List all the experimental procedures involved in details based on the information given in section
5.0. Make sure the experimental data obtained can be used to answer the objectives.

7.2 Week 2
7.2.2 Tasks
(i) Prepare the chemicals required for the calibration and experimental studies.
(ii) Carry out the calibration analysis and experimental studies based on the procedures prepared in
the previous week.
(iii) Tabulate the experimental data.

__________________________________________________________________________________
FKKSA/BKF3741/Module/Rev03092014
Module 1: BKF3741 Chemical Reaction Engineering Laboratory I

8.0 Report
The report should conform to the outline provided to you during the briefing session. Your grade
will depend to a great extent on following that outline closely. In addition to that, the following should be
included in the report:

1. Detailed derivation of equations required to determine the rate constant (refer to main reference as
given in the following section).
2. Determination of the rate constant of the reaction from the data obtained using the batch reactor.
Sample calculations are required.
3. Comparison of results obtained with the experimental data reported in the literature for similar
conditions.
4. Comments on the differences in the results obtained and discussion of the results and the quality
of the data and experimental procedures (difficulties and uncertainties).

9.0 References
H.S. Fogler, "Elements of Chemical Reaction Engineering"

__________________________________________________________________________________
FKKSA/BKF3741/Module/Rev03092014