THEORY

Plug flow reactors, otherwise called tubular reactors, comprise of a tube shaped pipe with
openings on each end for reactants and products to flow through. Plug flow reactors are
typically worked at steady state. Reactants are constantly expended as they stream down the
length of the reactor.
MATERIALS & APPARATUS

Materials
1. 0.25M Hydrochloric Acid, HCl
2. 0.1M Sodium Hydroxide ,NaOH
3. 0.1M Sodium Acetate, Na(Ac)
4. Deionized Water, H2O

Apparatus
1. Burette
2. Conductivity Meter
3. Plug Flow Reactor

METHODOLOGY

General Start Up
1. Ensure all the valves are initially closed except valves V4, V8 and V17.
2. The solutions are prepared for each experiment.
3. The power for the control panel is turned on.

Task Experiment 1 & 2 Experiment 3 & 4

B1 Deionized water 0.1M NaOH solution
B2 0.05M NaCl solution 0.1M Et(Ac) solution

4. The water jacket B4 and preheater B5 is filled with a clean water. The valves V13
and V18 is opened. Pump P3 is switch on to calculate the water through pre-heater
B5.
5. A stirrer motor M1 is switched on and the speed is set for about 200 rpm.
6. Valve V2, V4 and V10 is opened. Pump P1 is switched on. P1 is adjusted to flowrate
of 150 ml/min at flow meter, FI-01. Valve V10 is closed and pump P1 is switched off.
7. Valve V6, V8, V12 is opened. Pump P2 is switched on. P2 is adjusted to flow rate150
ml/min at flow meter FI-02. Valve V12 is closed and pump P2 is switched off.
8. The unit is now ready for the experiments.
Experiment 1 – Preparation of Calibration for Conversion vs. Conductivity
1. The following solutions are prepared:
 1 liter of sodium hydroxide, NaOH - .1M
 1 liter of sodium acetate, Na(Ac) – 0.1M
 1 liter of deionized water, H2O
2. The conductivity and NaOH concentration for each conversion values are determined
by mixing the following solutions into 100mL of deionized water:
 0% conversion : 100mL NaOH
 25% conversion : 75mL NaOH + 25mL Na(Ac)
 50% conversion : 50mL NaOH + 50mL Na(Ac)
 75% conversion : 25mL NaOH + 75mL Na(Ac)
 100% conversion : 100mL Na(Ac)

Experiment 2 - Back Titration for Manual Conversion Determination

1. The burette is filled up with 0.1M NaOH solution.
2. 10 ml of 0.25M HCl is measured in flask.
3. 50 ml of sample from the experiment is obtained and the sample is immediately added
to the HCl in the flask to quench the saponification reaction.
4. A few drops of pH indicator is added into the mixture.
5. The mixture is titrated with NaOH solution from the burette until the mixture is
neutralized. The amount of NaOH titrated is recorded.

Experiment 3 - Effect of Residence Time on the Reaction

1. The general start-up procedures are performed as above.
2. Valve V9 and V11 are opened.
3. Both NaOH and Et(Ac) solutions are allowed to enter the plug flow reactor R1 and
empty into the waste tank B3.
4. P1 and P2 are adjusted to give a constant flow rate of about 300ml/min at flowmeters
FI-01 and FI-02. Make sure that both flow rates are the same. The flow rates are
recorded.
5. The inlet (QI-01) and outlet (QI-02) conductivity values are being monitored until they
do not change over time. This is to ensure that the reactor has reached steady state.
 6. Both inlet and outlet steady state conductivity values are recorded. The concentration
of NaOH exiting the reactor and extent of conversion from the calibration curve is
obtained.
7. Optional : sampling valve V15 is opened and 50 ml of sample is collected. A back
titration procedure to manually determine the concentration of NaOH in the reactor and
extent of conversion is carried out.
8. The experiment steps 4 to 7 is repeated for different residence time by reducing the feed
flow rates of NaOH and Et(Ac) to about 250, 200, 150, 100 and 50 ml/min. Make sure
that both flow rates are the same.

General Shut Down

1. Pump P1, P2 and P3 is switched off. Valve V2 and V6 is closed.
2. The heaters is switched off.
3. The cooling water is kept circulating through the reactor while the stirrer motor is
running to allow the water jacket to cool down to a room temperature.
4. All liquid is drained from the unit by opening valve V1 to V19 if the equipment is not
going to be used for a long period of time.
5. The power is turned off for the control panel.