Chemical Engineering Lab- 2

Experiment-6

Group-5

Madhav Rathi (2018A1PS0723P)

Himanshu Chaturvedi (2018A1PS0031P)
Himanshu Singh (2018A1PS0025P)
Gaurav Bellal Natesh (2018A1PS0027P)
Avish Goel (2018A1PS0734P)

BITS Pilani
 Experiment 6
Isothermal Batch Reactor

1. Aim:
To determine the reaction rate constant (k) for the given saponification reaction of ethyl
acetate in aqueous sodium hydroxide solution.

2. Objective:
Study of a non-catalytic homogeneous reaction in a batch reactor.

3. Observations:
● 9.78 ml of ethyl acetate in 1 litre water
● 4g of NaOH in 1000ml water
● Volume of N/40 NaOH used for titration
At 60°C

S. No. Time (min) Volume of sample Volume of N/40 Sample taken Volume of N/40
taken (ml) HCl added to for titration NaOH used for
sample (ml) (ml) titration (ml)
1 5 10 20 30 6
2 10 10 20 30 7.7
3 15 10 20 30 8.2
4 20 10 20 30 9

At 70°C

S. No. Time (min) Volume of sample taken Volume of Sample taken Volume of N/40
(ml) N/40 HCl added for titration NaOH used for
to sample (ml) (ml) titration (ml)
1 5 10 20 30 7
2 10 10 20 30 7.9
3 15 10 20 30 8.3
4 20 10 20 30 8.7

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4. Sample Calculations:
Volume of N/40 HCl taken in flask= 20 ml

Volume of sample taken= 10 ml

Volume of N/40 NaOH used for titration= VNaOH

No. of moles of NaOH used = VNaOH*(1/40)*10-3 g.moles = 2.5 *10-5 * VNaOH g.moles

No. of moles of HCl present initially in flask= 20*(1/40)*10-3 g.moles

= 5*10-4g.moles

No. of moles of NaOH left in the sample = (5*10-4- VNaOH*2.5*10-5 )

CA= (5*10-4- VNaOH*2.5*10-5 )/ 10-2 g.mol/L

At 600C, For t= 5 min, VNaOH= 6 ml, CA = (5*10-4- 6*2.5*10-5 )/ 10-2 g.mol/L

= 0.035 g.mole/L

2
t (min) CA(g.mol/L) -ln(CA/CA0) 1/CA (L/g.mol)
5 0.035 1.049822124 28.57142857

10 0.03075 1.179280192 32.5203252

15 0.0295 1.220779923 33.89830508

20 0.0275 1.290984181 36.36363636

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t(min) CA(g.mol/L) -ln(CA/CA0) 1/CA(L/g.mol)
5 0.0325 1.123930097 30.76923077
10 0.03025 1.195674002 33.05785124

15 0.02925 1.229290612 34.18803419

20 0.02825 1.264076728 35.39823009

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5
Thus, (E/R) can be calculated from the graph of ln K vs 1/T:

k lnk T 1/T
0.4951 -0.7029955166 333.15 0.003001650908
0.3003 -1.202973304 343.15 0.002914177473

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5. ,Results and Discussions:

The below table shows the concentration of NaOH left in the sample for the 2 different
temperatures.

Reaction Temperature = 60 °C
Time (min)
Concentration of NaOH
left in the sample
5 0.035
10 0.03075
15 0.0295
20 0.0275

Reaction Temperature = 70 °C
Time (min)
Concentration of NaOH
left in the sample
5 0.0325
10 0.03025
15 0.02925
20 0.02825

As shown in the sample calculations, 2 models, one for a first order reaction and the other
for a second order reaction are fitted to the experimental data.

The plot for the second order reaction appears to be a marginally better fit than that for
the first order reaction. This can be observed by the R 2 value for the 2 plots. The second
order reaction fit has a R2 value of 0.9684 while that of the first order reaction fit has a R 2
value of 0.961.

Based on this, we can conclude that the saponification reaction is following 2nd order
rate kinetics based on whatever data was experimentally available.

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 Using the 2nd order rate kinetics equation, the value of the rate constant for the 2 reaction
temperatures were found out as follows:

Reaction Constant
(k) Reaction Temperature
0.4951 60 °C
0.3003 70 °C

The above table shows a strange trend. Theoretical expectations suggest that as the
temperature at which the reaction is carried out increases, the rate constant would also
increase. However, in this case the rate constant appears to decrease with increasing
temperature.

The activation energy of the reaction is found out to be -14.2011434 J/g.mol

A negative value of activation energy is not theoretically possible. This clearly indicates
the existence of several experimental errors during the performance of the experiment.
Either the temperatures were not adjusted properly or the titration was not done correctly.
It could also be possible that mistakes were made while noting the readings of the
experiment, which has resulted in this theoretically impossible result.

It is also possible that one of the data points was an outlier. That is, if the experiment was
performed for more data points, the outlier could have been removed, and better results
could have been obtained.

6. Conclusion:
➢ Based on the results and data analysis performed on the experimental data, we can
conclude that 2nd order rate kinetics best represents the kinetics of the given
saponification reaction.
➢ The rate constants of the reaction were calculated at 2 different temperatures, 0.4951 at
60 °C and 0.3003 at 70 °C. The decreasing trend of the rate constants with increase in
temperature was the first indication of the existence of experimental errors.

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➢ The activation energy is calculated from the rate constants and it comes out to be
negative (-14.2011434 J/g.mol). This is theoretically not possible as the activation energy
is a positive quantity and we are getting a negative value only due to the commission of
severe errors while performing the experiment.