ABSTRACT

In this experiment, we are using CSTR (model: BP143) is designed for experiment on chemical
reaction in liquid phase which have isothermal and adiabatic conditions. This model of CSTR
used consists of two tanks of solution (feed) and one reactor. More than that, it also has jacketed
reaction fitted in the agitated and condenser in this model complete with vessels for raw
materials and products, feed pump and thermostat. From
between sodium hydroxide and ethyl

this

experiment,

saponification

acetate can produce sodium acetate in a batch and the

CSTR will evaluate the rate data needed to design a bigger batch which is an industrial scale. To
simplify this experiment, two solution sodium hydroxide (NaOH) and ethyl acetate Et(Ac) was
put into its own feed tank and then reacted with each other in the CSTR. The product is then
analysed by the titrating the sample produce with 0.1 M sodium hydroxide to determine how
well the reaction go. Hence, the experiment was conducted and the results shows that the
significant value of conversion between sodium hydroxide and ethyl acetate increases almost
linearly with the increasing of residence of time.

INTRODUCTION
Continuous Stirrer-Tank Reactor (CSTR) usually runs under steady state condition with
continuous flow of reactant from the feed tank into the reactor to mix the reactant and form a
product. The inlet and outlet has the same significant value of composition as in the reactor. The
inlet and outlet streams rate inside of the reactor must be more reachable than any other reactors.
The inlet streams will bring all the reactants in at a particular rate and this stream will flow into a
large container where there is a shaft with a stirrer attached in the reactor that rotates around
continuously to mix the reactants. Hence, there is an outlet stream, which will let the solution to
exit from the reactor.
This CSTR (model: BP143) does not require much work to keep it running and due to its
simplicity of the components involved in the reactor, the maintenance is easy and cheap.
However, this reactor takes more space to mix the component compare to other reactor. In
reactor design, we have the exact size and type of reactor as well as the method of operation that
suitable for a given job. This may required the conditions in the reactor vary with the position
and time. In industrial sector, this modelBP:143 of CSTR is used when relatively small amount
of material are to be treated and this can be calculated with a proper integration of the rate of
equation for the operation.
However, this may cause some difficulties due to the temperature and composition of the
reacting fluid may varies from one point to another within the reactor. This depends on the
endothermic or exothermic nature of the reaction where the rate of heat addition or removal from
the system and the flow pattern of the fluid through the vessel. This can briefly indicates the
particular features and the main areas of application of these reactor types

OBJECTIVE

To carry out saponification reaction between Sodium Hydroxide (NaOH) and Ethyl

Acetate Et(Ac) by using continuous Stirred Tank Reactor (CSTR).

To determine the effect of residence time to the reactions extent of conversion.
To evaluate the reaction rate constant.

THEORY
Rate of Reaction and Rate Law
Simply put, rate of reaction can be roughly define as the rate of disappearance of reactants or the
rate of formation of products. When a chemical reaction is said to occur, a reactant diminishes
and a product produces, this is what constitutes a chemical reaction. For example:
aA+ bB

cC+ dD

A and B represent reactants while C and D represent products. In this reaction, A and B is being
diminished and C and D is being produced. Rate of reaction, concerns it with how fast the
reactants diminished or how fast the product id formed. Rate of reaction of each species
corresponds respectively to their stoichiometric coefficient. As such:
r A r B r C r D
=
= =
a
b
c d
The negative sign indicates reactants.
A usual equation for rA is:
r A=k C A C B
Where:
K = rate constant

= stoichiometric coefficient of A

CA = concentration of A species

= stoichiometric coefficient of B

CB = concentration of B species

Conversion
Taking species A as the basis, the reaction expression can be devided through the stoichiometric
coefficient of species A, hence the reaction expression can be arranged as follows:
b
c
d
A + B+ C + D
a
a
a
Conversion is an improved way of quantifying exactly how far has the reaction moved, or how
many moles of products are formed for every mole of A has consumed. Conversion XA, is the
number of moles of A that have reacted per mole of A fed to the system. As show below:
X A=

moles of A reacted
mole of A fed

Continuous Strirred Tank Reactor

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

F A 0F A + r A dV =
0

dN A
dt

Assumption:
Steady state, dNA/dt=0
Well-mixed throughout the reactor
Rearranging the generation, V = (FAoFA)/ -rA
In terms of conversion, 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 Distribution Function
Residence Time Distribution is a characteristic of the mixing that occurs in the chemical reactor.
There is no axial mixing in a plug flow reactor, and this omission can be seen in the residence
time distribution, RTD which is exhibited by this class of reactors. The continuous stirred tank
reactor is thoroughly mixed and its RTD is hugely different as compared to the RTD of PFR.

APPARATUS

The apparatus used in this experiment:

1.
2.
3.
4.

Conical flask
Measuring cylinder
Beakers
Burrette

PROCEDURE
General start-up Procedures:
1. The following solution were prepared:
i- 40L of sodium hydroxide, NaOH (0.1 M)
ii- 40 L of ethyl acetate, Et (Ac) (0.1M)
iii- 1 L of hydrochloric acid, HCl (0.25M) , for quenching.
2. All valves were initially closed.
3. The feed vessels were charged as follows:
i- The charge port caps for vessels B1 and B2 were opened.
ii- The NaOH solution was carefully poured into vessel B1 and Et (Ac) solution
was poured into vessel B2

iii- The charge port caps for both vessels were closed.
4. The power for control panel was turned on.
5. Sufficient water in thermostat T1 was checked. Refill as necessary.
6. The overflow tube was adjusted to give a working volume of 10L in the reactor R1.
7. Valves V2, V3, V3, V7, V8 and V11 were opened.8.The unit was ready for experiment.
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 let to
cooldown 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
7. Preparation Of Calibration Curve For Conversion Vs. Conductivity
a. The following solution were prepared:
i. 1 liter of sodium hydroxide, NaOH (0.1M).
ii. 1 liter of ethyl acetate, Et(Ac) (0.1M).
iii. 1 liter deionized water, H20.
b. The conductivity and NaOH concentration were determine for each conversion
values by mixing the following solutions into 100ml of deionized water:
i. 0% conversion 100 ml NaOH
ii. 25% conversion 75 ml NaOH + 25 ml Et(Ac)
iii. 50% conversion 50 ml NaOH + 50 ml Et(Ac)
iv. 75% conversion 25 ml NaOH + 75 ml Et(Ac)
v. 100% conversion 100 ml Et(Ac)
8. Back Titration Procedure For Manual Conversion Determination
a. Filled up burrette with 0.1M of NaOH.
b. 10 ml of 0.25M HCl in a flask was measured.
c. A 50 ml sample was obtain from the experiment and immediately added the
sample to the HCl in the flask to quench the saponification reaction.
d. A few drops of pH indicator were added to the mixture.
e. The mixture were titrated with NaOH till the solution changed color from
colorless to pink. The initial and final reading were recorded.
Experiment 1: Effect of Residence Time of The Reaction in a CSTR:
1. The general start-up procedures was 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 bout 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 rate 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.
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.

RESULT
PREPARATION OF CALIBRATION CURVE
Solution Mixtures

Conversion
(%)

H20

Concentratio
n of NaOH
(M)

Conductivity
(mS/cm)

0.1 M NaOH

0.1 M Et(Ac)

100

100

0.0500

9.780

25

75

25

100

0.0375

6.540

50

50

50

100

0.0250

3.960

75

25

75

100

0.0125

0.895

100

100

100

0.0000

0.207

Table 1.0: Table of preparation of calibration curve

Conductivity (mS/cm) vs Convertion (%)

60
50
40

Conductivity (mS/cm)

30
20
10
0
80

100

120

140

Convertion (%))

Figure 1: Graph Conductivity versus Conversion

TABLE FOR EXPERIMENT 1

160

180

200

No.

Temperature
(oc)

Flowrate of
NaOH
(ml/min)

Flowrate of
Et(Ac)
(ml/min)

Volume of NaOH (ml)

28.7

100

100

26.1

28.7

150

150

25.8

28.7

200

200

25.8

29.1

250

250

26.0

29.2

300

300

26.7

Residence time, ,
(min)

Conductivity
(Ms/cm)

Exit Concentration of
NaOH,
CNaOH (M)

Conversion, X, (%)

50.00

2.70

-2.2x10-9

100

33.33

2.72

-1.6x10-9

100

25.00

2.73

-1.6x10-9

100

20.00

2.74

-2.0x10-9

100

16.67

2.75

-3.4x10-9

100

Residence Time versus Conversion

60
50
40

Residence Time (min)

30
20
10
0
80

100

120

140

Conversion (%)

CALCULATION

160

180

200

F0= 0.1+0.1 = 0.2 L/min

Known quantities:
Volume of sample, Vs

= 50 ml

Concentration of NaOH in the feed vessel, CNaOH,f

= 0.1 mol/L

Volume of HCL for quenching, VHCl,s

= 10 mL

Concentration of HCl in standard solution, CHCls

= 0.25 mol/L

Volume of titrated NaOH, V1

= 9.8 mL

Concentration of NaOH used for titration, CNaOHs

= 0.1 mol/L

Concentration of NaOH that entering the reactor, CNaOH0.

CNaOHo= CNaOHf
= (0.1)
= 0.05 mol/L
Volume of unreacted quenching HCl,V2
V2= (CNaOH/ CHCls) x V1
= (0.1/0.25) x 26.1
= 10.44 mL
Volume of HCl reacted with NaOH in sample, V3
V3= VHCls V2
= 10 10.44
= -0.44
Moles of HCl reacted with NaOH in sample, n1
n1= (CHCls x V3) / 1000
= 0.25 x (-0.44)/1000
= -0.00011 mol
Moles of unreacted NaOH in sample, n2

n2= n1
= -0.00011 mol
Concentration of unreacted NaOH in the reactor, CNaOH
CNaOH = n2/Vs x 1000
= (-0.00011)/50 x 1000
= -2.2x10-9 mol/L
Conversion of NaOH in the reactor, X
X= (1- CNaOH/ CNaOHo) x 100%
= (1 (-2.2x10-9)/0.05) x 100%
= 100 %
Residence time,
=VCSTR / Fo
= 10 / 0.20
= 50 min
Reaction rate constant, k
k = (CAO CA) / CA2
= (0.05 (-2.29x10-9)) / (50 x (-2.29x10-9)2)
= 1.9069x1014 M-1min-1
Rate of reaction, -r A
-r A= kCA2
= 1.9069 x1014x (-2.2x10-9)2
= 9.99 x 10-4mol/L.min

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 graph 1, we can conclude that the conductivity is not consistent which are the
lines low down at 50% conversion which is the conductivity is 3.960 but then it keep on decrease
until 100%conversion. While for the second graph which is residence time versus conversion.
For this graph plotted, the residence time is remain constant to the conversion. The conversion
off residence time were recorded as 100%. As the residence time increase, the conversion also
increase but in this experiment there must be an error occur during conducting the experiment.
Firstly, the solution or solvent inside the fed tank must be contaminated due to left for too long
inside the tank. According to the lab technician, the solution were changed only once per
semester. Secondly, there must be error during preparing the sample for titration process and also
present of parallex error during taking the reading of titration process. This may be lead to error
in calculation percentage of conversion. There is no possibilities for a reactor to archive 100%
conversion as there may be some defect during undergoes the experiment.
For the saponification process, it is one kind of process to make a soap. Saponification
process is 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.
RECOMANDATION
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.
REFERANCE
1. http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_06.htm
2. http://www.wisegeek.com/what-is-a-calibration-curve.htm
3. http://www.engin.umich.edu/~cre/asyLearn/bits/cstr/index.htm