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OPERATING PROCEDURES
General Start-Up Procedures for Experiments 3 & 4
1) Ensure that all valves are initially closed except valves V4, V8 and V17.
2) Prepare the following solutions:
a. 20 liter of sodium hydroxide, NaOH (0.1 M)
b. 20 liter of ethyl acetate, Et(Ac) (0.1 M)
c. 1 liter of hydrochloric acid, HCl (0.25 M), for quenching
3) Fill the feed tank B1 with the NaOH solution and feed tank B2 with the Et(Ac) solution.
4) Fill the water jacket B4 and pre-heater B5 with clean water.
5) Turn on the power for the control panel.
6) Open valves V2, V4, V6, V8, V9 and V11.
7) Switch on both pumps P1 and P2. Adjust P1 and P2 to obtain flow of approximately 300 ml/min at
both flow meters FI-01 and FI-02. Make sure both flow rates are the same.
8) Allow both solutions to flow through the reactor R1 and overflow into the waste tank B3.
9) Open valves V13 and V18. Switch on pump P3 to circulate the water through pre-heater B5. Switch
on stirrer motor M1 and set the speed to about 200 rpm to ensure homogeneous water jacket
temperature.
10) For experiment 4, perform the following additional steps:
a. Switch on the heaters.
b. Open valve V19 to let the cooling water to flow through the cooling tubes. Adjust valve V19
to obtain reasonable cooling water flow in order to minimize the temperature overshoot at
the TIC-01 during heater cut-off.
c. Set the temperature setpoint on TIC-01 to the desired temperature.
11) The unit is now ready for experiment.
General Shut-Down Procedures
1) Switch off both pumps P1, P2 and P3. Close valves V2 and V6.
2) Switch off the heaters.
3) Keep the cooling water circulating through the reactor while the stirrer motor is running to allow the
water jacket to cool down to room temperature.
4) If the equipment is not going to be used for long period of time, drain all liquid from the unit by
opening valves V1 to V19. Rinse the feed tanks with clean water.
5) Turn off the power for the control panel.
CPE554
EXPERIMENT PROCEDURES
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
The following procedures will calibrate the conductivity measurements of conversion values for the reaction
between 0.1 M ethyl acetate and 0.1 M sodium hydroxide:
PROCEDURES:
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