PROCEDURES:

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 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:
i- 1 L of sodium hydroxide, NaOH (0.1M)
ii- 1 L of sodium acetate , Et (Ac) (0.1M)
iii- 1 L of deionised water, H2O.
2. The conductivity and NaoH concentration for each valu were determined by mixing the
following solution into 100 mL of deionised water.
i- 0% conversion : 100 mL NaOH
ii- 25% cinversion : 75 mL NaOH + 25 mL Et (Ac)
iii- 50% conversion : 50 mL NaOH + 50 mL Et (Ac)
iv- 75% conversion : 23 mL NaOH + 75 mL Et (Ac)
v- 100% conversion : 100 mL Et (Ac)
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 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 njust 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 id 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.

APPARATUS:
1. Continuous stirred tank reactor. Model: BP 143
2. 50 mL burette
3. 200 mL beaker
4. Conical flask
6. Conductivity probe
7. 100 mL measuring cylinder.
MATERIAL:
0.1 M Sodium Hydroxide, NaOH
0.1 M Ethyl Acetate, Et(Ac)
0.1 M Hydrochloric Acid, HCl
De-ionised water
Phenolphthalein

SOLTEQ-QVF Continuous Stirred Tank Reactor (Model: BP 143)

RESULT
Experiment 1: Effect of residence time of the reaction in a cstr

Reactor volume: 4L
Concentration of NaOH in feed vassel: 0.1M
Concentration of Et(Ac) in feed vassel: 0.1M
Flow
rate
Of
NaOH
(L/min)
0.10
0.15
0.20
0.25
0.30

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

0.10
0.15
0.20
0.25
0.30

Total
flowrate
, F0
(mL/mi
n)
0.20
0.30
0.40
0.50
0.60

Reside
nce
time,
(min)

Conducti
vity
(mS/cm)

Exit
concentra
tion of
NaOH,
CNaOH (M)

Conversi
on, X (%)

20.0
13.33
10.0
8.0
6.67

a) Preparation of Calibration Curves

Conversion

Solution Mixtures
0.1 M NaOH

0%
25 %
50 %
75 %
100 %

100 mL
75 mL
50 mL
25 mL
-

0.1 M Et
(Ac)
25 mL
50 mL
75 mL
100 mL

100
100
100
100
100

mL
mL
mL
mL
mL

Concentration of HCl: 0.25M

1
2
3
4
5

Conductivit
y (mS/cm)

0.0500
0.0375
0.0250
0.0125
0.0000

13.92
9.87
6.38
2.89
0.1073

H2O

Back titration for manual conversion determination:

Sample

Concentrati
on of NaOH
(M)

Volume Of NaOH titrated

(mL)
24.0
25.5
26.0
25.8
25.8

Calculation
1) F0 = 0.1+0.1 = 0.2 L/min
Volume of sample, Vs = 50 mL
Concentration of NaOH in the feed vessel, C NaOH,f = 0.1 mol/L
Volume of HCL for quenching, VHCl,s = 10 mL
Concentration of HCl in standard solution, C HCls = 0.25 mol/L
Volume of titrated NaOH, V1= 9.8 mL
Concentration of NaOH used for titration, CNaOHs = 0.1 mol/L

i- Concentration of NaOH that entering the reactor, C NaOH0.

CNaOHo = CNaOHf
= (0.1)
= 0.05 mol/L
ii- Volume of unreacted quenching HCl,V2
V2 = (CNaOHs / CHCls) x V1
= (0.1/0.25) x 22
= 8.8 mL
iii- Volume of HCl reacted with NaOHin sample, V3
V3 = VHCls V2
= 10 8.8
= 1.20
iv- Moles of HCl reacted with NaOH in sample, n1
n1 = (CHCls x V3) / 1000
= 0.25 x 1.2/1000
= 0.0003 mol
v- Moles of unreacted NaOH in sample, n 2
n2 = n 1
= 0.0003 mol
vi- Concentration of unreacted NaOH in the reactor, C NaOH
CNaOH = n2/Vs x 1000
= 0.0003/50 x 1000
= 0.006 mol/L

vii- Conversion of NaOH in the reactor, X

X = (1- CNaOH / CNaOHo) x 100%
= (1 0.006/0.05) x 100%
= 98.8 %

viii- Residence time,

= VCSTR / Fo
= 10 / 0.20
= 50 min
ix- Reaction rate constant, k
k = ( CAo CA) / CA2
= ( 0.05 0.006) / (50 x 0.0062)
= 24.44 M-1 min -1
x- Rate of reaction, -rA
-rA = kCA2
= 24.44 x 0.0062
= 8.79 x 10 -4 mol/L.min