OPEN ENDED LAB

Experiment no 16

AIM: To determine the reaction rate constant for saponification of ethyl-acetate with NaOH at
ambient conditions.

THEORY: In an ideal CSTR (that is an ideal steady state flow reactor) the contents in the reactor
are well mixed and have uniform composition throughout. Thus the exit stream has the same
composition as the fluid within the reactor. This type of reactor is also known as MIXED FLOW
REACTOR.

Reactor volume (volume of fluid in the reactor) = VR, Liters, Volumetric feed rate (volumetric feed
rate of A + volumetric feed rate of B) =V0 , LPM Space time =  = VR / Vo, min

The performance equation for the mixed flow reactor at steady state is:

XA & rA are evaluated at exit stream conditions, which are the same as the conditions within the
reactor.
DESCRIPTION:
The reactor is made up of SS -304. The air compressed feed reactants are given through Rotameter.
The concentration of feed and the products coming out from the reactors are analyzed by chemical
titration and check the effect and the performance of the reactor. A Continuous stirred tank flow
reactor (CSTR) required. 6 No. 50 cc graduated cylinder. No. 100 cc titration flasks, 50 cc burette and
one stopwatch, conductivity Cell (optional).

CHEMICALS:
1. N/10 NaOH,

2. N/10 HCI,

3. N/10 Ethyl acetate (8.8 gms of ethyl acetate in 1 L of water),

4. Indicator (Phenolphthalein)

UTILITIES REQUIRED:
1. Compressed Air Supply at 2 Bar, 0.5 CFM.

2. Water Supply.

3. Drain.

4. Electricity Supply: 1 Phase. 220 V AC. 0.5 kW.

5. Instruments. Laboratory Glassware and Chemicals required for analysis as per the system adopted.

SPECIFICATIONS:
Reactor : Material Stainless Steel 304 Grade, Capacity 2 Ltrs (Approx).

Stirrer : Stainless Steel 304 Grade Impeller and shaft coupled with FHP Motor

Feed Tank (2Nos.) : Material Stainless Steel 304 Grade. Capacity - 20 Ltrs.

Feed Circulation : By compressed air

Flow Measurement : Rota meter 2Nos. (one each for Reactants)

Piping : Stainless Steel 304 Grade and PVC

Pressure Regulator : 0-2 Kg/cm2

Pressure Gauge : Bourdon type 0-2 Kg/cm2

Stop Watch : Electronic

The whole unit is assembled rigidly on a base plate and mounted on a stand. Most of the parts are
powder coated and rests are painted with auto paints.

PROCEDURE:
Prepare 20L of N/10 NaOH solution by dissolving 80 gm of NaOH in 20L of water.

1. Prepare 20L of N/10 ethyl acetate solution by mixing 176 gms of ethyl acetate in 20L of water.

2. Fill the respective tanks with these solutions.

3. Adjust the flow rate of the two streams so that in the feed mixture CAo = CBo i.e. have equal flow
rates (e.g. 2 LPH each you may use the flow range: 2 LPH to 16 LPH for each stream) using calibrated
rotameters.

4. Pass equimolar feed rates of ethyl acetate and NaOH into the CSTR by allowing equal volumetric
feed rates of reactants in to the reactor and simultaneously start the mixer of the CSTR. Ensure
constant stirring throughout the experiment.

5. After about 10 min or time equal to the residence time of the reactor (whichever is greater) i.e.
when steady state is achieved, collect sample of the liquid at the out let.

6. Titrate this solution against N/40 HCl (add HCl from burette).

7. Using phenolphthalein as indicator, note the volume of N/40 HCl used (VHCl)

8. Note the volumetric flow rate of liquid at the end of the reactor.

9. Note the reaction temperature.

10. For calculating the conversion at equilibrium condition, collect the sample 10 ml, in an empty
conical flask and allow the reaction to proceed for completion for two hours. After two hours titrate
the solution with N/10 HCI using phenolphthalein as indicator. Note the volume of N/10 HCI used.

11. Repeat all the steps for four to six different flow rates of feed. Note: report k at the reaction
temperature
2

PRECAUTION:
1. Measure the exact volume of water and weigh the chemicals.

2. Always use clean water and good quality chemicals and standard solution for titration.

3. Use electronic balance for weighing of chemicals. Don't mix the droppers of different chemicals.

4. Keep close all the drain valves and vent valve should open while tilling the reactant in feed tanks.

5. Flow should not be disturbed during the experiments. 6. Handle the chemicals carefully

TROUBLE SHOOTING:
1. If any type of suspended particles come in the Rota meter. Remove the Rota meter clean the
tube and fit again at its place.
2. If there is any leakage; tight that part or remove that and refix that again after wrapping
Teflon tape.
3. If Rota meter fluctuating more than average tight control knob of that. (Procedure: two nuts
are there lose first nut and tight the second slightly, and then first also. Both nuts are on Rota
meter)

Conclusion:
In conclusion, the reaction rate constant for the saponification of ethyl acetate with
sodium hydroxide at ambient conditions was successfully determined. The experimental
results confirmed that the reaction follows a second-order kinetic model, where the rate
depends on the concentrations of both ethyl acetate and sodium hydroxide. The
calculated rate constant aligns with the expected values for similar conditions,
demonstrating the effectiveness of the method used. Overall, the experiment provided a
practical understanding of reaction kinetics and the factors influencing the rate of
saponification.