ADAMSON UNIVERSITY

Ermita, Manila
College of Engineering
Chemical Engineering Department

UNIT OPERATIONS 2 LABORATORY

Experiment No. 7
Measurement of Reaction Conversion

Submitted by:

Aquino, Chamylle Rose T.

Carlos, Fauline Deune G.
Dela Guardia, Islie D.S.
Tayactac, Honeylet R.
Salazar, Allen Grace A.

Submitted to:

Engr. Robert E. Delfin

May 9, 2019
 I. OBJECTIVES

1. To determine the degree of conversion of the reactants mixed in a flask at certain

time.
2. To determine the degree of conversion of the reaction for a given set of condition of
the continuous stirred-tank reactor.

II. MATERIALS/ EQUIPMENTS NEEDED

1. Continuous Stirred-tank Reactor

2. 1 L glass flask and stopper
3. 2- 10 mL pipette
4. 2- 50 mL burette
5. Phenolphthalein indicator
6. 250 ml of standardized 0.1 M NaOH
7. 250 mL of standardized 0.1 M EtOAc
8. Timer
9. 100 mL of 0.1 m HCL
10. 40 g solid caustic soda
11. 99 mL pure ethyl acetate
12. 20 L distilled water

III. EQUIPMENT SET-UP

Figure III-A- Glass flask with stopper

 Figure III-B- Continuous Stirred-tank Reactor

IV. PROCEDURE

Part A: Reaction in a Flask

1. Mix 250 mL of standardized 0.1 M NaOH and 250 mL of standardized 0.1 M EtOAc in 1
L flask and secure stopper.
2. After say 20 minutes of mixing, take 10 mL sample and place in the titration flask.
3. Quench this sample with 10 mL of 0.1 M HCl then add phenolphthalein indicator.
4. Titrate this mixture with 0.1 M NaOH until end point is reach. Note volume used.
5. Repeat steps 2 – 4 after 10 minutes, 20 minutes, and 30 minutes of mixing.
Fig. IV-A.1. Mixing 250 mL standardized 0.1 M NaOH Fig. IV-A.2. Titrating the mixture
with and 250 mL of standardized 0.1 M EtOAc 0.1 M NaOH until end point is reach.

Fig. IV-A.3. End point of each mixture after

10, 20, and 30 minutes.
Part B: Reaction in a CSTR Reactor

1. Preparation of reactants
a) Caustic soda: Place 2.5 liters of 0.1 M solutions in Tank A. Make this solution up
wearing safety goggles and gloves and standardize it by titration with 0.1 M HCl
b) Ethyl acetate: This is very volatile and flammable liquid and should be kept away
from naked lights. For a similar 0.1 M solution the amount of EtOAc needed is
(molecular weight x 10 liters / 10 / density = 88/10/0.89) 99 ml for 10 liters of
solution in preferably de-ionized or distilled water Tank B.
 2. Set up the temperature control unit and allow the temperature of the reactor to reach 30°C
with the stirrer on.
3. Switch on both pumps. Adjust flow rates to 0.10 liters/min for each feed and check that
the product discharges to the sump tray.
4. After 20-30 minutes when the reactor has reached a steady state note the following
readings.
a. Flowrates of NaOH and EtOAc
b. Outlet temperature T,°C
5. Take a 10ml at reactor outlet and NaOH inlet tank and analyze for caustic soda
concentration.
6. Titrate the mixture.

Fig. IV-B.1. Reacting Caustic soda and Ethyl acetate with Fig. IV-B.2. Titrating the mixture
its corresponding temperature and flow rate until end point is reach.

V. DATA AND RESULTS

 Mixing in a flask

Sample Time(minutes) Conc. Of NaOH (M) % Concentration

1 10 0.0426 53.76

2 20 0.0444 55.56

3 30 0.0375 62.5
  Reaction in a Continuous Stirred-tank Reactor

Sample Conc of NaOH Conc of NaOH Conc of NaOH

In Tank A at the Inlet of at the Outlet of % Conversion
the Reactor the Reactor

1 0.1M 0.0496M 0.03M 39.52

2 0.1M 0.05M 0.02M 60

3 0.1M 0.05M 0.01M 80

SAMPLE COMPUTATION:

Mixing in a Flask

V1 = 8.6mL, V2 = 8mL, V3 = 6mL

0.1𝑚𝑜𝑙 1𝐿
𝑛= 8.6𝑚𝐿 = 8.6𝑥10−4 𝑚𝑜𝑙
𝐿 1000𝑚𝐿
8.6𝑥10−4 𝑚𝑜𝑙
𝐶𝑎 = = 0.0462𝑀
1𝐿
8.6 + 10 𝑚𝐿 1000𝑚𝐿
0.1 − 0.0426
𝑥= 100 = 53.76%
0.1
Reaction in a Continuous Stirred-tank Reactor

Flowrates: Volume Titration:

A1= 49.7mL; A2 = 50.5mL; A3 = 50.6mL S1 = 7mL; S2 = 8mL; S3 = 9mL

B1= 50.5mL; B2 = 50.3mL; B3 = 50.5mL

Conc A in Inlet

𝐹𝑎 49.7
𝐶𝑎 = 𝐶𝑖 = 0.1 = 0.0496𝑀
𝐹𝑎 + 𝐹𝑏 49.7 + 50.5
0.1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1𝑚𝑜𝑙 𝐻𝐶𝑙 1000𝑚𝐿 𝐻𝐶𝑙
𝑈𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑 𝐻𝐶𝑙 = 7 𝑚𝐿 𝑁𝑎𝑂𝐻 ( )
1000𝑚𝐿 𝑁𝑎𝑂𝐻 1𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 0.1𝑚𝑜𝑙 𝐻𝐶𝑙

𝑈𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑 𝐻𝐶𝑙 = 7 𝑚𝐿 𝐻𝐶𝑙

𝑅𝑒𝑎𝑐𝑡𝑒𝑑 𝐻𝐶𝐿 = 10𝑚𝐿 𝐻𝐶𝐿 − 7 𝑚𝐿 𝐻𝐶𝑙 = 3 𝑚𝐿 𝐻𝐶𝑙

 0.1𝑚𝑜𝑙 𝐻𝐶𝑙
1𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
3 𝑚𝐿 𝐻𝐶𝑙
𝑂𝑢𝑡𝑙𝑒𝑡 𝐶𝑜𝑛𝑐. 𝑁𝑎𝑂𝐻, 𝐶𝐴𝑜 = 1000𝑚𝐿 𝐻𝐶𝑙 1𝑚𝑜𝑙 𝐻𝐶𝑙
1𝐿
10𝑚𝐿 𝑠𝑎𝑚𝑝𝑙𝑒 1000𝑚𝐿

𝑂𝑢𝑡𝑙𝑒𝑡 𝐶𝑜𝑛𝑐. 𝑁𝑎𝑂𝐻, 𝐶𝐴𝑜 = 0.03 𝑚𝑚𝑜𝑙

100 (𝐶𝐴𝑖 − 𝐶𝐴𝑜 )

% 𝐶𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛, 𝑋 =
𝐶𝐴𝑖

100 (0.0496 𝑀 − 0.03 𝑀)

% 𝐶𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛, 𝑋 =
0.0496 𝑀

% 𝐶𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛, 𝑋 = 39.52 %

VI. CONCLUSION

The purpose of this experiment is to measure the reaction conversion with the use of flask as
batch reactor and CSTR to achieve the objectives. The students conclude that conversion is
increased proportionally with residence time. This proved that when flow rate increases, the
reaction rate constant becomes smaller and the rate of reaction becomes higher. The reaction
conversion decreases with increase in reactants flow rate and this is because of decrease of
residence time. Also, increase of reactor volume also has positive effect on the conversion and
specific rate constant. Conversion and rate constant increase with an increase in volume. Specific
rate constant and conversion increase must be linear with temperature to meet the objectives of
the experiment. The complexity of a continuous stirring tank reactor still reflects a direct
proportionality between the residence times versus the conversion.

A higher conversion on the CSTR would be observed compared to batch reactor due to the
increased surface contact between the reactants that is enhanced by the stirring. The agitation
also helps in distributing uniform composition and temperature within the system. The rate law
of the reaction is also dependent to the concentrations of the NaOH and EtOAc since the said
saponification process follows a second-order reaction.

For future researchers, a better analysis of the behavior of a saponification process in a flask and
in a CSTR would be the inclusion and variation of other parameters. For minimal errors, careful
executions of procedures when preparing the reagents would be efficient in attaining higher
accuracy. Also, when reading the volume, the position of the eye must be perpendicular to the
reading scale of burette and graduated cylinder. Additionally, apparatuses should be washed
before using so that any chemical out into it will not react with any others chemical and to ensure
that it is not contaminated. Lastly, make sure the valves are closed and there is no any leak from
the reactor to make sure it will run appropriately. The color that obtained in titration must be
same for entire experiment to avoid any variation in result.
VII. APPENDIX

Appendix A. Experimental Data

 Mixing in a Flask

Standard Solution Volume of

Sample Volume of
NaOH Back
Sample volume Quench HCl
HCl (M) NaOH (M) Titer
(mL) (mL)
(mL)
1 20 0.1 0.1 8.6 0
2 20 0.1 0.1 8 0
3 20 0.1 0.1 6 0

 Reaction in Continuous Stirred-tank Reactor

From the feed tank

Standard Solution Volume of

Sample Volume of
NaOH Back
Sample volume Quench HCl
HCl (M) NaOH (M) Titer
(L) (mL)
(mL)
1 5 0.1 0.1 10 0
2 5 0.1 0.1 10 0
3 5 0.1 0.1 10 0

From the exit sample point

Standard Solution Volume of

Sample Volume of
NaOH Back
Sample volume Quench HCl
HCl (M) NaOH (M) Titer
(L) (mL)
(mL)
1 10 0.1 0.1 7 0
2 10 0.1 0.1 8 0
3 10 0.1 0.1 9 0