INTRODUCTION

Reactor is one of equipment used mostly in the industrials sector. It changes the raw material
into the desired product. A good reactor will give a high production and economical. One
of criteria to choose or to design a good reactor is to know the effectiveness of the reactor
itself. There a many types of reactor depending on the nature of the feed materials and
products. One of the most important we need to know in the various chemical reaction was
the rate of the reaction. The continuous stirred-tank reactor (CSTR) which is also known
as vat or back-mix reactor usually is a common ideal reactor type in chemical engineering.
A CSTR often refers to a model used to estimate the key unit operation variables when
using a continuous agitated-tank reactor to reach a specified output. This reactor works for all
fluids, liquids, gases, and slurries. The behavior of a CSTR is always modeled by that of a
Continuous Ideally Stirred Tank Reactor (CISTR). All calculations performed with CISTRs
assumed perfect mixing.
In a perfect mixed reactor, the output composition is identical to the material inside the
reactor, which is a function residence time and rate of reaction. CSTR used in this experiment,
(model: BP 143) is designed for students experiments on chemical reaction in liquid phase
under adiabatic and isothermal conditions. CSTR consists of two tanks of solutions and one
reactor.
The reactor is modeled in order to perform the saponification reaction between sodium
hydroxide and ethyl acetate. Saponification reaction of ethyl acetate and sodium hydroxide
produced sodium acetate in batch and the continuous stirred tank reactor evaluate the rate data
needed to design a production scale reactor.

OBJECTIVES
The main purposes of conducting this experiment are :

to carry out saponification reaction between Sodium Hydroxide, NaOH and Ethyl
Acetate, Et(AC) by using a Continuous Stirred Tank Reactor, CSTR
to determine the effect of residence time to the reaction's extent of conversion
to evaluate the reaction rate constant

THEORY
Rate of equation and rate law
The rate of reactions or speed of reaction for a reactant and products in particular reactions
can be defined as how fast or slow the reaction takes place. For examples is about the
oxidation process between iron under the atmospheric is undergoes a slow reaction compare
to the combustion of butane in a fire that can be categories as fast reaction. Consider the
chemical reaction as below:
aA + bB

pP + qQ

The lowercase letter which are a, b, p, and q refer to the stoichiometric coefficient while the
capital letter which are A, B, P and Q refer to the reactants and products.
According to the IUPACs Gold Book definition the rate of reaction, r in the chemical reaction
is occur in a closed system which is under a constant volume conditions, without build up of
reaction intermediates, is defines as:
r=

1 d [ A ] 1 d [B ] 1 d [ P] 1 d [Q]
=
=
=
a dt
b dt
p dt
q dt

Where [A], [B], [P] and [Q] are referred to the morality of the substances. Based on IUPAC
the times must be in second and the rate of reaction is in a positive sign. The mass balance for
any system in general is:
IN - OUT + GENERATION -CONSUMPTION= ACCUMULATION
Mass is a conservative entity, hence given a control volume V the sum of mass flows entering
the system will be equal to the sum exiting minus the consumed or accumulated fractions.

Continuous Stirred Tank Reactors (CSTR)

CSTR runs at steady state with continuous flow of reactants and products; the feed assumes a
uniform composition throughout the reactor, exit stream has the same composition as in
the tank.
General Mole Balance Equation
V

F A 0F A + r A dV =
0

dN A
dt

Assumptions
Steady state, therefore dNA/dt = 0
Well-mixed therefore is the same throughout the reactor.
Rearranging the generation,
In terms of conversion,

V = (FAo - FA)/ -rA

X = (FAoFA) / FAo
V = (FAoX) / -rA

A calibration curve is a method used in analytical chemistry to determine the concentration of

an unknown sample solution. It is a graph generated by experimental means, with
the concentration of solution plotted on the x-axis and the observable variable, for example,
the solutions absorbance plotted on the y-axis. The curve is constructed by measuring the
concentration and absorbance of several prepared solutions, called calibration standards. Once
the curve has been plotted, the concentration of the unknown solution can be determined by
placing it on the curve based on its absorbance or other observable variable.
Residence Time
The reactors residence time is defined as the reactor volume divided by the total feed flow
rates.
3

Residence time,

V CSTR
F0

MATERIAL AND APPARATUS

The unit Continuous Stirred Tank Reactor Model BP143 comes complete with a jacketed
glass reactor, constant temperature water circulating unit, vapor condenser, individual reactant
feed tanks and pumps, temperature and conductivity measuring sensors, and of course, data
acquisition system. Apart from that, there were also some laboratory apparatus involved such
as:

Burette
conical flask
measuring cylinder
ph indicator
beakers

Among the chemicals used are:

0.1 M Sodium Hydroxide, NaOH

0.1 M Ethyl Acetate, Et(Ac)
0.1 M Hydrochloric Acid, HCl
De-ionized water

PROCEDURE
General start-up Procedures:
1. The following solution were prepared:
i40L of sodium hydroxide, NaOH (0.1 M)
ii40 L of ethyl acetate, Et (Ac) (0.1M)
iii1 L of hydrochloric acid, HCl (0.25M), for quenching.
2. All valves were initially closed.
3. The feed vessels were charged as follows:
iThe charge port caps for vessels B1 and B2 were opened.
iiThe NaOH solution was carefully poured into vessel B1 and Et (Ac) solution was poured into
vessel B2.
iiiThe charge port caps for both vessels were closed.
4.
5.
6.
7.

The power for control panel was turned on.

Sufficient water in thermostat T1 was checked. Refill as necessary.
The overflow tube was adjusted to give a working volume of 10L in the reactor R1.
Valves V2, V3, V3, V7, V8 and V11 were opened.8.

The unit was ready for experiment.

Back Titration Procedures for Manual Conversion Determination:
1. A burette was filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl was measured in a flask.
3. A 50 mL sample was obtained from the experiment and immediate the sample was added to the HCl
in the flask to quench the saponification reaction.
4. A few drops of pH indicator were added into the mixture.
5. The mixture was titrated with NaOH solution from the burette until the mixture was
neutralized. The amount of NaOH titrated was recorded.
Effect of Residence Time of Reaction in a CSTR:
1. The general start-up procedures were performed.
2. Pump 1 and pump 2 were switched on and valves V5 and V10 were opened to obtain the highest
possible flow rate into the reactor.
3. The reactor was filled up with both of the solution until it is just about to overflow.
4. Valves V5 and V10 were readjusted to give a flow rate of about 0.1 L/min. the flow rate
for both valves must be same. The flow rates were recorded into a data.
5. The stirrer M1 was switched on and the speed was set about 200 rpm.
6. The conductivity value at Q1 was started monitoring until it does not change over time.
This is to ensure that the reactor has reached steady state.
7. The steady state conductivity value was recorded and the concentration of NaOH and
extent of conversion in the reactor was found out from the calibration curve.
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8. Sampling valve V12 was opened and 100mL of sample was collected. It directly proceed
with the back titration procedures to manually determine the concentration of NaOH in
the reactor and extent of conversion.
9. The experiments was repeated (steps 5-9) for different residence times by adjusting the
feed flow rate of NaOH and Et(Ac) to about 0.15, 0.20, 0.25, and 0.30 L/min. the flow
rate for both must be same.

General shut-down Procedures:

1. The cooling water valve V13 was kept open to allow the cooling water to continue flowing.
2. Pumps P1 and pumps P2 were switched off. Stirrer M1 was switched off.
3. The thermostat T1 was switched off. The liquid in the reaction vessel R1 was left to cool down to room
temperature.
4. Cooling water V13 was closed.
5. Valves V2, V3, V7, and V8 were closed. Valves V4, V9 and V12 were opened to drain
any liquid from the unit.
6. The power for control panel was turned off
Preparation of Calibration Curve for Conversion vs Conductivity:
1. The following solution were prepared:
i1 L of sodium hydroxide, NaOH (0.1M)
ii1 L of sodium acetate , Et (Ac) (0.1M)
iii1 L of de-ionized water, H2O.
2. The conductivity and NaoH concentration for each value were determined by mixing the following
solution into 100 mL of de-ionized water.
i0% conversion : 100 mL NaOH
ii25% conversion : 75 mL NaOH + 25 mL Et (Ac)
iii50% conversion : 50 mL NaOH + 50 mL Et (Ac)
iv75% conversion : 23 mL NaOH + 75 mL Et (Ac)
v100% conversion : 100 mL Et (Ac)

RESULTS
Table 1: Preparation of Calibration Curve

Conversion

Solution Mixtures
0.1 M NaOH 0.1 M Et(Ac)

0%
25 %
50 %
75 %
100 %

100 mL
75 mL
50 mL
25 mL
-

25 mL
50 mL
75 mL
100 mL

H2O
100 mL
100 mL
100 mL
100 mL
100 mL

Concentratio
n of NaOH
(M)
0.0500
0.0375
0.0250
0.0125
0.0000

Conductivity
(mS/cm)
7.66
5.40
2.90
1.30
0.157

Table 2: Tabulated data

Temperature

()

Flow rate
of NaOH
(mL/min)

Flow rate
of Et(Ac)
(mL/min)

Total flow
rate of
solutions,
F0
(mL/min)

Residence
time,

28.0
28.2
28.3
28.4
28.6

0.1
0.15
0.20
0.25
0.30

0.1
0.15
0.20
0.25
0.30

0.2
0.3
0.4
0.5
0.6

50
33.33
25
20
16.66

Conductivit
y (mS/cm)

Exit
concentratio
n of NaOH,
CNaOH (M)

Conversion
, X (%)

Volume
of NaOH
(mL)

2.01
1.91
1.84
1.75
1.74

0.004
0.004
0.0036
0.004
0.004

92
92
92.8
92
92

28.0
28.0
28.2
28.0
28.0

(min)

9
8
7
6
5
Conductivity (mS/cm)

4
3
2
1
0
0%

20%

40%

60%

80%

100%

120%

Conversion, X (%)

Figure 1: Calibration Curve

93
92.8
92.6
92.4
Conversion, X(%)

92.2
92
91.8
91.6
91.4
10

15

20

25

30

35

40

45

50

55

Residence Time (min)

Figure 2: The Conversion of NaOH against Residence Time

SAMPLE CALCULATION
Volume of sample, VS = 50 mL
Concentration of Initial NaOH, CA0 = 0.1 mol/L
Volume of HCL, VHCl = 12 mL
Concentration of HCl, CHCl = 0.25 mol/L
Volume of NaOH titrated, V1 = 28.0 mL
i-

ii-

iii-

iv-

vvi-

vii-

viii-

Concentration of NaOH entering the reactor

CNaOH0
= CA0
= (0.1 mol/L)
= 0.05 mol/L
Volume of unreacted HCl
V2 = (CNaOH/ CHCl) x V1
= (0.1 mol/L / 0.25 mol/L) x 28 mL
= 11.2 mL
Volume of reacted HCl
V3 = VHCl-V2
= 12 mL 11.2 mL
= 0.08 mL
Mole of reacted NaOH
n1 = (CHCl x V3) / 1000
= 0.25 x 0.08 / 1000
= 0.00008 mol
Mole of unreacted NaOH
n2 = n1
= 0.00008 mol
Concentration of unreacted NaOH in Reactor
CNaOH
= n2/VS x 1000
= 0.00008/ 50 x 1000
=0.004 mol/L
Conversion of NaOH in reactor
X = (1- CNaOH / C NaOH0) x 100%
= (1- 0.004 / 0.05) x 100%
= 92%
Residence time

=V
/F
CSTR

ix-

= 10 / 0.2
= 50 min
Rate reaction constant

k = (CA0 CA)/
CA2
= (0.05 -0.004) / 50 (0.004)2
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DISCUSSION
According to the experiment that had been conducted, we need to achieve three objectives
which are to carry out the saponification process between NaOH and Et (Ac) in a CSTR
reactor, to determine the effect of the residence time onto the reaction extent of conversion and lastly to
determine the constant rate of reaction. From the data collected, two graph had been plotted
which are conductivity versus conversion and residence time versus conversion. From the
Figure 1, we can conclude that the conductivity is consistently slows down throughout the overall
conversion. The second graph is residence time versus conversion. For this graph it could be
seen that the residence time is increased proportionally at average 92% conversion. But there
are certain fluctuate peak which due to the error that may be affects the result and graph.
Saponification process is the process to make soap. It takes place in a continuous reaction.
In this experiment, the reaction of saponification is quenching with hydrochloric acid to stop
the reaction. The reaction rapidly reacts in increasing of experiment. Back titration is done to
investigate if the reaction is stop .As the result for rates of constant is not correspond to the
theory, thus there are some errors occurred during this experiment such as while taking the
reading of the burette the position of the eyes is not at the same level of the meniscus. So, to improve the
reading and get the better results, the positions of the eyes must be parallel to the meniscus.
Besides, we have to rinse all the apparatus before we use it. This is to ensure that all the
beakers, or burette is clean so that any chemical that we put into these apparatus does not
react with any others chemicals. By doing all these precaution, we can get more accurate
reading and thus improve the results.
CONCLUSION
Based on the objectives of this experiment, which is to determine the residence time onto the
reaction extent of conversion, the relationship conversion and residence time was directly proportional. But
the reaction rates constant were determined for all varies flow rate. From the calculated data, the
rate constant of reaction is increasing when the conversion is higher. We can conclude that the
experiment was successfully conducted since we get the right conclusion.

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RECOMMENDATION
1. Make sure reactor does not have any leaks and valve closed and opened as needed, controlled the valve
carefully and slowly when adjusting the flow rate to obtain 0.10 L/min. It is to make sure flow rate
will stabilize and the experiment will run smoothly.
2. Repeat titrations two or three times because a lot of error comes from titration or use
another method other than titration.
3. Divide into two teams which is the first team in charge of the CSTR 40 liters machine
while the second team would carry out the back titration procedures.
4. Take conductivity reading when the conductivity not changes in time because it can change rapidly in
short of time.
5. Make sure CSTR 40 liters machine is running appropriately, it to prevent harm to the machine and
individual that used the machine.

REFERENCES
1. Sulivan, J. A. (1960). Fluid Power Theory and Application., 2nd ed., Reston Publishing
Company, Reston, VA.
2. Salmi, T. O., et. al. (2011). Chemical Reaction Engineering and Reactor Technology.,
Taylor & Francis Group, CRC Press, Boca Raton.
APPENDICES

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