FACULTY OF CHEMICAL ENGINEERING

UiTM Terengganu, Bukit Besi Campus

Program : Diploma in Chemical Engineering
Course : Introduction To Chemical Reaction
Engineering
Course Code : CHE244
Lecturer : Marshahida bin Mat Yashim



Laboratory Report

Experiment Title
THE SAPONIFICATION REACTION OF ETHYL ACETATE, ET(AC) AND
SODIUM HYDROXIDE, NAOH

No Name Student ID No Signature
1. MOHAMAD TURMIZI BIN JAAFAR
2013450634
2. AMIRUL AIMAN BIN ZULFAKAR
2013419606
3. MUHAMMAD AZIZI BIN AB WAHAB
2013451738
4. NUR SYAFIQAH BINTI MOHD SAIDI
2013884596
5. NOR SYAZA MUNIERAH BINTI SALLEH
2013246812


Date of Experiment : 03.09.2014
Date of Submission : 23.09.2014
Received by:-

________________________
MARSHAHIDA BINTI MAT YASHIM
Date :



List of contents
THE SAPONIFICATION REACTION OF ETHYL ACETATE, ET(AC) AND SODIUM
HYDROXIDE, NAOH ........................................................................................................................... 1
1.0 INTRODUCTION ...................................................................................................................... 5
2.0 OBJECTIVE ............................................................................................................................... 7
3.0 APPARATUS ............................................................................................................................. 8
4.0 THEORY .................................................................................................................................. 11
5.0 PROCEDURE ........................................................................................................................... 13
7.0 DISCUSSION ........................................................................................................................... 18
8.0 CONCLUSION ......................................................................................................................... 19
Bibliography ......................................................................................................................................... 21





















List of figures
Figure 1 : Cross-sectional diagram of Continuous stirred-tank reactor .................................................. 5
Figure 2 : Single Continuous Stirred Tank Reactors (CSTRs) ............................................................... 6
Figure 3 : Continuously Stirrer Tank Reactor (CSTR) in series ............................................................. 6
Figure 4 : 25 mL burette ......................................................................................................................... 8
Figure 5 : Stand with clamps .................................................................................................................. 8
Figure 6 : Conical Flask .......................................................................................................................... 9
Figure 7 : Continuous Stirred Tank Reactor 40L .................................................................................... 9
Figure 8 : 100 ML Beaker ..................................................................................................................... 10
Figure 9 : Calibration curve (Conversion vs. Conductivity) ................................................................. 16
Figure 10 : Graph of conversion against residence time ....................................................................... 16




















List of tables
Table 1 : Calculations for back titration ................................................................................................ 12
Table 2 : Preparation calibration curve ................................................................................................. 15
Table 3 : Effect of residence time Continuous Stirred Tank Reactor ................................................... 15

























TITLE : THE SAPONIFICATION REACTION OF ETHYL ACETATE, ET(AC) AND
SODIUM HYDROXIDE, NAOH
1.0 INTRODUCTION

Firstly, a common type of reactor is the mixing, or stirred reactor .The basic components
of this device will include a mixer or agitator mounted to a tank. One of the stirred reactors is
Continuous Stirred Tank Reactors (CSTR). The flow stirred tank reactor in series is a
common reactor type in environmental applications. The principle characteristic is that the
reactor is assumed to be instantaneously and perfectly mixed. Majority of industrial chemical
processes, a CSTR reactor is the equipment in which raw materials undergo a chemical
change to form desired product. The types of process this equipment is the continuous stirred
tank reactor which is this reactor is almost always operated at steady state. The CSTR reactor
used are most commonly used in industrial processing, primarily in homogeneous liquid-
phase flow reactions, where constant agitation is required. They may be used by themselves,
in series, or in a battery. It is referred to as the continuously stirred tank reactor (CSTR). It is
normally operated at steady state and is assumed to be perfectly mixed. The characteristic of
this equipment is run at steady state with continuous flow of reactants and products, the feed
assumes a uniform composition throughout the reactor, and exit stream has the same
composition as in the tank.


Figure 1 : Cross-sectional diagram of Continuous stirred-tank reactor



The CSTR can run as single reactor and also in series. The CSTR reactor is connected
in series so that the exit stream of one reactor is the feed stream for another reactor. There are
three reactor vessels connected in series by piping, each containing a propeller agitator driven
by a variable speed electric motor and the unit based on the simplest classic case of well
mixed, multi-staged process operation. The solution in each reactor is well stirred and the
concentration can be measured. These three reactors are to compare the measured responses
of the vessel concentrations to deliberate change at the inlet with a theoretical prediction.


Figure 2 : Single Continuous Stirred Tank Reactors (CSTRs)

The piping arrangement has been designed to include a dead time coil in the system. Feed
liquid to the first vessel is drawn from of the two sump tanks by a pump, via a flow meter and
control valve. The trace material concentration in each sump tank is made to be different. At
a selected instant, a sudden change from one feed to the other is made: either for continuous
period is known as the step function, or for a short interval is known as impulse function, and
the concentration or conductivity changer with time in each vessel is measured.


Figure 3 : Continuously Stirrer Tank Reactor (CSTR) in series



The advantages of CSTR are easily maintained, good temperature control, cheap to construct,
reactor has large heat capacity and interior of reactor is easily accessed. Meanwhile, the
disadvantages of using CSTR are lowest conversion per unit volume and also by-passing and
channelling possible with poor agitation.
2.0 OBJECTIVE

That shown the objective of this experiment:
i) To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
ii) To determine the effect of residence time onto the reaction extent of conversion..
iii) To determine the reaction rate constant.
































BURETTE
BASE
CLAMP
SCALE
LIQUID
HOLDER

3.0 APPARATUS

A.









B.














Figure 4 : 25 mL burette
Figure 5 : Stand with clamps




C.










Figure 6 : Conical Flask

D.

Figure 7 : Continuous Stirred Tank Reactor 40L


SCALE



E.

Figure 8 : 100 ML Beaker
















4.0 THEORY

One of the organic chemical reactions known to ancient man was the preparation of soaps
through a reaction called saponification. Natural soaps are sodium or potassium salts of fatty
acids, originally made by boiling lard or other animal fat together with lye or potash
(potassium hydroxide). Hydrolysis of the fats and oils occurs, yielding glycerol and crude
soap. In the industrial manufacture of soap, tallow (fat from animals such as cattle and sheep)
or vegetable fat is heated with sodium hydroxide. Once the saponification reaction is
complete, sodium chloride is added to precipitate the soap. The water layer is drawn off the
top of the mixture and the glycerol is recovered using vacuum distillation.
The equation below shows the saponification process between sodium hydroxide and ethyl
acetate (irreversible reaction) to produce sodium acetate and by-product ethanol.

NaOH + C
2
H
5
O
2
CCH
3
CH
3
CO
2
Na + H
3
CCH
2
OH
Sodium Hydroxide Ethyl Acetate Sodium Acetate Ethanol

A. Preparation of Calibration Curve for Conversion vs. Conductivity

The reaction to be studied is the saponification reaction of ethyl acetate Et(Ac) and
sodium hydroxide (NaOH). Since this is a second order reaction, the rate of reaction
depends on both concentrations of Et (Ac) and NaOH. However, for analysis
purposes, the reaction will be carried out using equimolar feeds of Et (Ac) and NaOH
solutions with the same initial concentrations. This ensures that both concentrations
are similar throughout the reaction.

NaOH + Et (Ac) Na(Ac) + EtOH

It will calibrate the conductivity measurement of conversion values for the reaction
between 0.1 M ethyl acetate and 0.1 M sodium hydroxide that we will get from the
experiment.






B. Back Titration for Manual Conversion Determination

It is advisable to carry out manual conversion determination on experiment samples to
verify the conductivity measurement values. It is based on the principle of quenching
the sample with excess acid to stop any further reactions, then back titrating with a
base to determine the amount of unreacted acid.

NaOH + HCl NaCl + H
2
O


The calculations of back titration :


No. Quantities Formula Unit
1. Concentration of NaOH entering
the reactor, C
NaOH,0

C
NaOH,f

mol/L
2. Volume of unreacted quenching
HCL, V
2

(C
NaOH,s
/C
HCL,s
) x
V
1
mL
3. Volume of HCL reacted with
NaOH in sample, V
3
V
HCL,S
V
2
mL
4. Moles of HCL reacted with NaOH
in sample, n
1
(C
HCL,S
x V
3
) /
1000
mol
5. Moles of unreacted NaOH in
sample, n
2
n
1
mol
6. Concentration of unreacted NaOH
in the reactor, C
NaOH
n
2
/ V
s
x 1000 mol/L
7. Conversion of NaOH in the
reactor, X
[1 (C
NaOH
/
C
NaOH,0
)] x 100%


Table 1 : Calculations for back titration


C. Reaction Rate Constant












5.0 PROCEDURE

1. Preparation of Calibration Curve for Conversion vs. Conductivity

i) The solutions for the first method were prepared
- 1 L of sodium hydroxide, NaOH ( 0.1 M )
- 1 L of sodium acetate, Et (Ac) ( 0.1 M )
- 1 L of deionised water, H
2
O


ii) The conductivity and NaOH concentration had been determined for each
conversion values by mixing the solutions into 100 mL of deionised water :

- 0% conversion : 100 mL NaOH
- 25% conversion : 75 mL NaOH + 25 mL Et (Ac)
- 50% conversion : 50 mL NaOH + 50 mL Et (Ac)
- 75% conversion : 25 mL NaOH + 75 mL Et (Ac)
- 100% conversion : 100 mL Et (Ac)


2. Back Titration for Manual Conversion Determination

i) 0.1 M NaOH solution was filled in a burette.
ii) 10 mL of 0.25 M HCL was measured in a flask.
iii) 50 mL sample had been obtained from the experiment and had been added up to
the HCL in the flask immediately to quench the saponification reaction.
iv) A few drops of pH indicator were added into the mixture.
v) The mixture had been titrated with NaOH solution from the burette until the
mixture is neutralized and the amount of NaOH titrated was recorded.

3. Reaction Rate in the CSTR

i) The general start-up procedures as before were performed.
ii) Both pumps P1 and P2 were switched on simultaneously and valves V5 and V10
were opened to obtain the highest possible flow rate into the reactor.
iii) The reactor had been filled up with both the solution until it is just about to
overflow.
iv) The valves V5 and V10 were readjusted to give flow a rate of about 0.1 L/min.
Both flow rate were made at the same value and it had been recorded.
v) The stirrer M1 was switched on and the speed was set up about 200 rpm.


vi) The conductivity value was started to be monitored at Ql-401 until it does not
change over time. This is to ensure that the reactor has reached steady state.
vii) The steady state conductivity value was recorded and the concentration of NaOH
in the reactor was obtained and extent of conversion from the calibration curve.
viii) Sampling valve V12 was opened and a 50 mL sample was collected. Back
titration procedure was carried out to manually determine the concentration of
NaOH in the reactor and extent of conversion.
ix) The experiment was repeated (step 5 to 9) for different residence times by
adjusting the feed flow rates of NaOH and Et (Ac) to about 0.15, 0.20, 0.25, 0.30
L/min. Both flow rates were make sure to be the same.






















6.0 RESULT



Table 2 : Preparation calibration curve




Reactor volume : 40 L
Conc. of NaOH in feed vessel : 0.1 M
Conc. of Et(Ac) in feed vessel : 0.1 M

No Temperature
(C)
Flow rate
of NaOH
(mL/min)
Flow rate
of Et
(Ac)
(mL/min)
Total
flow rate
of
solutions,
F
0

(mL/min)
Residence
time,
(min)
Conductivity
(mS/cm)
Exit
concentration
of NaOH,
C
NaOH
(M)
Conversion,
X (%)
1. 27.0 100 100 200 200.00 3.30 0.002 96
2. 27.1 150 150 300 133.33 3.14 0.004 92
3. 27.3 200 200 400 100.00 3.00 0.005 90
4. 27.5 250 250 500 80.00 2.90 0.006 88
5. 27.7 300 300 600 66.67 2.78 0.008 84

Table 3 : Effect of residence time Continuous Stirred Tank Reactor


Conversion Solution
Mixtures
Concentration
of NaOH (M)
Conductivity
(mS/cm)
0.1 M
NaOH
0.1 M
Et(Ac)
H
2
O
0% 100 mL - 100 mL 0.0500 5.930
25% 75 mL 25 mL 100 mL 0.0375 2.160
50% 50 mL 50 mL 100 mL 0.0250 1.619
75% 25 mL 75 mL 100 mL 0.0125 0.757
100% - 100 mL 100 mL 0.0000 0.0900




Figure 9 : Calibration curve (Conversion vs. Conductivity)




Figure 10 : Graph of conversion against residence time







CALCULATION

NaOH + HCl NaCl + H
2
O


Sample calculations for flow rate = 0.10 L/min

Volume of sample, V
s
= 50 mL

Concentration of NaOH in the feed vessel, C
NaOH,f
= 0.1 M

Volume of HCl for quenching, V
HCl,s
= 10 mL

Concentration of HCl in standard solution, C
HCl,s
= 0.25 mol/L

Volume of NaOH titrated, V
1
= 24.0 mol/L

Concentration of NaOH used for titration, C
NaOH,s
= 0.1 mol/L

Concentration of NaOH entering the reactor, C
NaOH,0
= (1/2)(0.1)
= 0.05 mol/L

Volume of unreacted quenching HCl, V
2
= (C
NaOH,s
/C
HCl,s
) x V
1

= (0.1/0.25) x 24.0
= 9.6 mL

Volume of HCl reacted with NaOH in sample, V
3
= V
HCl,s
- V
2

= 10 9.6
= 0.4 mL

Moles of HCl reacted with NaOH in sample, n
1
= (C
HCl,s
x V
3
)/1000
= (0.25 x 0.4) / 1000
= 0.0001mol

Moles of unreacted NaOH in sample, n
2
= n
1
= 0.0001 mol

Concentration of unreacted NaOH in the reactor, C
NaOH
= n
2
/ V
s
x 1000
=

x 1000
= 0.002

Conversion of NaOH in the reactor, X = (1 -

) x 100%
= (1 -

) x 100%
= 92%

Residence time, = V
CSTR
/F
0

= 40 L/ (0.10 + 0.10) L/min
= 200 min


7.0 DISCUSSION


The experiment is conducted to determine the reaction rate and to determine the effect
of the residence time on the conversion in Plug Flow Reactor which related with it. The
CSTR model is used to predict the behaviour of chemical reactors, so that the key reactor
variables, which is the dimensions of the reactor, can be estimated.


The experiment is conducted by setting the flow rate of both solutions NaOH and
Et(Ac) into 0.10 L/min, 0.15 L/min, 0.20 L/min, 0.25 L/min and 0.30 L/min at each run of
experiment. From the experiment, the residence time is about to decrease when the flow rates
of the reactor become faster. Residence time is the removal time which is the average amount
of time that a particle spends in a particular system. Furthermore, residence time is measured
with the amount of substance which is present in the system.

When using the residence time equation, it is significant to made a variety of
assumptions. It is assumed that chemical degradation does not occur in the system in question
and that particles do not attach to surfaces that would hinder their flow. If chemical
degradation were to occur in a system, the substance that originally entered the system may
react with other existing compounds in the system, causing the residence time to be
significantly shorter since the substance would be chemically broken down and effectively be
removed from the system before it was able to naturally flow out of the system

Therefore, when the residence time decrease, it indicates that less molecules of
reactants are reacted with each other. Thus, the conversion of reactant into product is
decrease. From the result, it shows that when the flow rates was set into 0.30 L/min for both
reactants which is the highest flow rate in this experiment; the residence time of that reactants
in the CSTR is the shortest which is 66.67 min and give out the result for conversion of
84.0%.
Oppositely, when the flow rate for both reactants was set into 0.10 L/min which is the
lowest flow rate, the residence time of those reactants in the CSTR is the longest which is 200
min and the highest conversion of the reactants is 96.0 %. While for flow rates of 0.15 L/min,
0.20 L/min and 0.25L/min; the residence time are 133.33 min, 100.00 min and 80.00 min
respectively and the conversion of reactants are 92.0 %, 90.0 % and 88.0 % respectively.






8.0 CONCLUSION

The purpose of this experiment is to carry out saponification reaction between NaOH
and Et(Ac) in a CSTR which also required to determine the effect of residence time onto
the reaction extent of conversion and to determine the reaction rate constant. Continuous
stirred tank reactor is used in this experiment in order to achieve the purpose of this
experiment. After completing the experiment, we are able to collect the data and all the
purposes are achieved. From the results, it shows that each of the flow rates increase from
0.10 L/min to 0.30 L/min, the conversion of NaOH decrease from 96% to 84%. The
graph shows that conversion of NaOH versus residence time is plotted. It is directly
proportional. As the conversion decrease, the residence is decrease as well.
There are a few recommendations that can improve the experiment result. With these
recommendations, the result would be more better than before. This experiment is
considered succeed as all the purposes are achieved.



















9.0 RECOMMENDATIONS

1. The device needs to be well maintenance in order to avoid it from malfunctioning
during the experiment period like the one we are having in our session.

2. To get a better result, only one person is needed to take care of the opening and
closing of the valve and other person take care of the pump. This is because some
valve needed to be opened or closed simultaneously.

3 Make sure the tank is filled with the correct solution and to the correct amount.
Different substance reacts differently and lack of substance can damage the apparatus.

4 Make sure general start-up procedure is done first in order to check the machine
functionality.


5 The burette should be rinsed with sodium hydroxide after rinsed using the distilled
water.
















10.0 REFERENCES


Bibliography
A.James. 2014. [Online] 19 September, 2014. [Cited: 01 June, 2012.]
http://en.wikipedia.org/wiki/Saponification.
M.Rone. 1975. [Online] 18 July, 1975. [Cited: 7 May, 1975.]
http://www.sciencedirect.com/science/article/pii/0009250976850580.
Wojes, Rayan. 2014. A.Datum. [Online] 5 May, 2014. [Cited: 23 september, 2014.]
http://iitkgp.vlab.co.in/?sub=35&brch=107&sim=1175&cnt=1.