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Objective:: Feed Tanks Batch Reactor

This experiment determined the rate constant for the saponification reaction of ethyl acetate with NaOH via titrimetry. Equimolar concentrations of ethyl acetate and NaOH were added to a batch reactor. Samples were taken over time and back titrated to calculate concentrations and determine the rate constant. The saponification reaction follows second order kinetics. Results were recorded in tables and graphs, showing the inverse of concentration decreasing over time with a rate constant that differed slightly from experimental values, possibly due to side reactions or errors.

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860 views

Objective:: Feed Tanks Batch Reactor

This experiment determined the rate constant for the saponification reaction of ethyl acetate with NaOH via titrimetry. Equimolar concentrations of ethyl acetate and NaOH were added to a batch reactor. Samples were taken over time and back titrated to calculate concentrations and determine the rate constant. The saponification reaction follows second order kinetics. Results were recorded in tables and graphs, showing the inverse of concentration decreasing over time with a rate constant that differed slightly from experimental values, possibly due to side reactions or errors.

Uploaded by

fareeha saeed
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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OBJECTIVE:

Determination of rate constant for saponification of ethyl acetate with NaOH via titrimetry
followed by integral analysis using stoichiometric proportions.

ABSTRACT:
This experiment was performed to observe the rate constant values at different time intervals.
For this purpose, a batch reactor was used in which equimolar concentrations of ethyl acetate and
sodium hydroxide were added. After sometime, known volume of unknown concentration of
mixture was taken. Then it was back titrated against sodium carbonate molar solution. Hence,
concentrations of mixture were calculated and results were recorded in the form of tables and
graphs and the calculated value was being compared with the experimental one.

APPARATUS:
Glass wares (beakers, conical flasks, burettes, pipettes), magnetic stirrer.

REAGENTS:
Distilled water, standard HCL solution, standard Na2CO3 solution, standard NaOH solution,
methyl orange indicator, standard ethyl acetate solution.

INTRODUCTION:
A batch reactor is a closed system with no continuous flow of reactants entering the system or
products leaving the system while the reaction takes place. In batch reactors, a reaction mixture
can react for long time in order to reach high conversions. Batch reactors can be operated as
static or mixed. Mixing helps remove concentration gradients and provides shear, while mass
transfer will be by both convection and diffusion. Static batch are poorly mixed, do not induce
shear and rely on diffusion for mass transfer. Batch reactors are closed systems that operate
under unsteady-state conditions. High conversions can be obtained by leaving reactants in
reactor for extended periods of time. Batch reactor jackets allow the system to change heating or
cooling power at constant jacket heat flux. It is good for producing small amounts of products
while still in testing phase and easy to clean. Batch reactors are mostly used in the fermentation
of beverage products, waste-water treatment etc. (Wilderer, Irvine et al. 2001)

Feed tanks

Batch reactor
Peristaltic pump

Figure 1: Labelled diagram of batch reactor


THEORY:
The saponification reaction is the hydrolysis of an ester with basic conditions to produce an
alcohol and the sodium salt of carboxylic acid. This term is mostly used in order to identify
reaction which occurs in the alkaline condition with a fat to convert into soap. So, the hydrolysis
of ethyl acetate to produce the sodium salt of acetic acid and ethyl alcohol with caustic soda is
called as saponification reaction, but in this case the final product is not soap. (Terry and
Stieglitz 1927)

REACTION KINETICS:
The reaction mechanism for the saponification reaction is given as follows:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
Saponification of ethyl acetate is a second order
reaction. Hence, the rate law becomes:

For stoichiometric proportions


CA = C B
Hence, integrated rate law becomes
1/CA = 1/CAO + kt

PROCEDURE:
 1000 ml (0.06 M) standard solutions of HCL, NaOH and ethyl acetate were being
prepared.
 1000 ml standard solution of Na2CO3 (0.03 M) was being prepared.
 500 ml of ethyl acetate and NaOH were being dumped in batch reactor and stirring was
started.
 10 ml sample after every five mintues was being withdrawn and the concentration of
NaOH in sample was determined via back titration.
OBSERVATIONS & CALCULATIONS:
Initial concentration of NaOH in reactor (CAO) = 0.06/2 = 0.03 M
TABLE # 1: CONCENTRATION OF NaOH AT DIFFERENT TIME INTERVALS:

CA (mol/dm3) 1/CA (dm3/mol) Time (t) (min)


0.012 83.33 5
0.024 41.67 10
0.042 23.81 15
0.054 18.52 20
0.066 15.15 25
0.072 13.89 30

TABLE # 2: AMOUNT OF Na2CO3 USED VIA BACK TITRATION AT DIFFERENT


TIME INTERVALS:

Time (t) (min) Amount of Na2CO3 used (ml)


5 13
10 11
15 8
20 6
25 4
30 3

Na2CO3 + 2HCL 2NaCL + CO2 + H2O


BACK TITRATION CALCULATIONS:
Na2CO3 : HCL
2M1V1 = M2V2
2x0.03x13/0.06 = V2
13ml = V2 (Amount of free acid left after neutralization with mixture)
V (Amount of acid used by mixture) = Total acid added – V2
V = 15 ml – 13 ml
V = 2 ml
Mixture : HCL
M1V1 = M2V2
M1 (Concentration of mixture in unknown sample) = 0.06x2/10 = 0.012M
CA = 0.012M
Same calculations can be done for other readings.
GRAPH OF TIME VERSUS INVERSE OF CONCENTRATION OF MIXTURE IN
UNKNOWN SAMPLE:

90

80

70

60
1/CA (dm3/mol)

50

40

30
f(x) = 1.04 x
20

10

0
0 5 10 15 20 25 30 35
Time (min)

DISCUSSION & CONCLUSION:


As it is evident from the graph that with the passage of time, the inverse of concentration of
mixture is decreasing. The value of slope is 1.0358 while the value of CAO turns out to be 0.67
M. It can be seen that the calculated value of initial concentration of mixture is greater as
compared to the experimental value. There could be a lot of reasons such as occurrence of side
reactions, faulty apparatus, inadequate knowledge of observer, loss of some amount of sample
during back titration or wrong calculations during molar solution preparations etc.

REFERENCES:
1. Terry, E. M. and J. Stieglitz (1927). "The Coefficient of Saponification of Ethyl Acetate by Sodium
Hydroxide." Journal of the American Chemical Society 49(9): 2216-2222.
2. Wilderer, P. A., et al. (2001). Sequencing batch reactor technology, IWA publishing.

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