CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

1.0

Ethyl Acetate

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SUMMARY
The objective of this experiment are to measure the rate constant of the reaction between

ethyl acetate and sodium hydroxide under batch reaction and to study the liquid phase reaction
kinetics in batch reactor.This experiment was conducted by preparing 3 different solution which
are 1 L of sodium hydroxide,NaOH (0.1M),250mL of ethyl acetate,Et(Ac)(0.1M) and 250mL of
hydrochloric acid,HCl (0.1M).200mL of 0.1M ethyl acetate was pipetted into a clean dry conical
flask.Another 200mL of 0.1M sodium hydroxide (NaOH) was placed into 500mL beaker.20mL
of 0.1M hydrochloric acid was pipetted into 11 different conical flask which label 1 to 11.Ethyl
acetate and the sodium hydroxide were mixed using the mixture for 5 minutes, then 20mL of the
solution was pipetted into conical flask 1. 3 drops of phenolphthalein were added for further
titration.From the result obtained,three graph were plotted in order to find the value of rate
constant, k using two different method which are integrated rate law and half life method.From
graph 1/CA against time the value of k obtained is 12.729.For the other graph which CA vs time,
the value of k obtained is 3.13 by using the half life method.

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

2.0

Ethyl Acetate

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DATA AND RESULTS

Concentration of

Time

Flask

(min)

Number

Amount of
NaOH titred
(mL)

NaOH,
CNaOH (M)

Conversion,
X (%)

1/CA

(Self
calculate)

0.05

20

11.5

0.0425

15

23.53

Of

10

12.2

0.039

22

29.41

Sodium

15

13.6

0.032

36

37.04

20

14.4

0.028

44

43.48

25

15.3

0.0235

53

54.05

30

15.8

0.021

58

64.52

35

16.6

0.017

66

83.33

40

17

0.015

70

100

50

17.6

0.012

76

142.86

60

10

18

0.01

80

111.11

70

11

18.8

0.006

88

166.67

Hydroxide (NaOH)
M1V1= M2V2
(0.1 mol/ L) (200mL) = (M2) (400mL)
M2= 0.05 mol/L
CA0= 0.05mol/L

a. CA0

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

NaOH concentration in 20 mL sample from the reactor

20 Y
0.1

mol / mL
1000
20
=

Let Y = Amount of NaOH titred (ml)

Conversion,X

X= CNaOH(t=0) - CNaOH(t) x 100%

CNaOH(t=0)

Ethyl Acetate

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CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

Ethyl Acetate

Graph 1 : Conversion,X vs Time

Graph 2 : 1/CA vs TIME

* From the graph the value for the K obtained is 12.729

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CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

Ethyl Acetate

Graph 3 CA vs Time
t1/2= Time when the concentration of NaOH is half converted
Half of NaOH converted= 0.05 mol/L 2
= 0.025 mol/L
Based on the graph:
y = -0.0038X + 0.0493
0.025 = -0.0038X + 0.0493
X = 6.39 min

k= 1/ t1/2 . CA0
= 1/ (6.39 0.05)
= 3.13
3.0

ANALYSIS AND DISCUSSION

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CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

Ethyl Acetate

P a g e |6

The objective of this experiment is to measure the rate constant of the reaction between ethyl
acetate and sodium hydroxide under batch condition ,and study the liquid phase reaction kinetics
in a batch reactor. This experiment were run by preparing 1 L of sodium hydroxide, NaOH (0.1
M) , 250 mL of ethyl acetate, Et(Ac) (0.1 M) ,and 250 mL of hydrochloric acid, HCl (0.1 M).
Then 11 sample of 20ml HCl been pipette into conical flask and added 3drops of phenolphthalein
and 200ml of Et(Ac) been poured into 200ml of NaOH. The mixture then been stirred and every
5minute the 20ml of mixture been pipetted into the conical flask containing the 20ml HCl . Then
the sample was titrated with NaOH. The result was tabulated at table 1.
Then, the concentration of NaOH was obtained by calculation using M1V1=M2V2 and the
conversion was calculated. Graph 1 is about the conversion against time which plotted using the
data obtain in the table 1. This graph shows that conversion increases as the time increase. The
graph 2 is about the reciprocal concentration against time with an equation y= 12.729X - 9.74,
the graph suppose to be a straight line graph. So, in this experiment there might be some error
when preparing the solution that may affect the graph. From this graph, we obtain the value of
rate constant ,k = 12.729 and this is called Integrated rate law method. Graph 3 is concentration
against time and this graph is ascending with an equation y= -0.0038X +0.0493 . From the graph
we calculate the half-time of NaOH concentration which is 0.025mol/L. We obtain the half-time
concentration by dividing the initial concentration which is 0.05mol/L by half. The half-life that
we calculated is 6.39 min from the equation. From the value of half-life ,we able to calculate the
rate constant by using this formula k= 1/ t1/2 X CA0 which is called half-life method. The value of
rate constant that we obtain was k= 3.13 .
As we obtain the value of rate constant for each method, the values are different for each
method because rate constant for half-life method is calculated based on time of the
concentration reduce to half of its initial value while the integrated rate law method use plotted
graph 2 to get the gradient of the line which equal to rate constant. Since our graphs were not
straight line so the value of rate constant might differ from the theoretical value.

4.0

CONCLUSIONS AND RECOMMENDATIONS

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

Ethyl Acetate

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CONCLUSIONS
By referring to the Graph 1 of Conversion,X (%) against time,t (min), the graph shows
that conversion increases as time increases. Theoretically, the graph will show as time increases,
the conversion increases. The graph also shows that the highest conversion value occurs at time
70 min which is 88.0% while the lowest conversion value occurs at time 0 min with conversion
0 %. In the Graph 2 of 1/

CA

against time,t(min) were plotted, the slope of the graph is

increasing. 1/CA shows the lowest value which is 20 M-1 at time 0 min and highest value at time
70 min which is 166.67 M-1.Theoretically, value of 1/

CA

is increase as time increase which

this experiment is same according to the theory. From the Graph 3 of CA (M) versus time,t (min),
it shows that the slope is decreasing with increase of time. The graph shows at time 0 min, the
concentration of NaOH (M) is at the highest of 0.05 M while at time 70 min, the concentration of
NaOH (M) is the lowest which is 0.006 M. The concentration of NaOH is decrease due to the
increase of amount of NaOH is titrated. The half of NaOH converted is 0.025 mol/L , the t1/2
which time when the concentration of NaOH is half converted is 6.39 min. The reaction rate
constant for this experiment is 3.13 L/mol.min.

RECOMMENDATIONS
There are many recommendations to improve the result obtain and to avoid some error
during the experiment. First, the solutions should be prepared correctly before run the
experiment. Next, make sure the timer is set to 5 minutes as soon the HCl solution contact with
Et(Ac) solution in order to obtain accurate data. Make sure the apparatus is clean and rinsed up
with distilled water before used it so that no impurities or excess chemical from previous
experiment is mix with our solution. Lastly, during pipetting the solution, the persons eye who
takes the reading should be parallel and same level with the pipette so that there is no parallax
error. Last but not least, the pipette need to replace so that no leaking occurred or the pipette
should be service so that the scale can be seen.

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

5.0

Ethyl Acetate

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TUTORIAL
1. It is vital to conduct certain chemical reaction in bench scale up. It is to understand the
potential waste streams. To examine macro-processes, process interaction, process
variations, process controls and development of standard operation procedure. It helps for
a better understanding of the overall process including the side processes. With these
information, it helps to build the information base so that the technology can be permitted
and safely implemented.
2. Based on a journal article, this is a study of direct synthesis of hydrogen peroxide by
using batch reactor. The direct synthesis of hydrogen peroxide from molecular hydrogen
and oxygen on a supported palladium catalyst was studied at 258297 K in a laboratoryscale batch reactor. The catalyst was in the form of finely dispersed slurry in
methanol/CO2 to suppress the internal and external mass transfer resistances.
Experiments carried out under kinetic control revealed that hydrogen peroxide was
successfully formed on the catalyst surface, but it was hydrogenated as the reaction time
was prolonged. The mass balances of the components were considered in detail and a
reaction mechanism was proposed, based on the competitive adsorption of hydrogen and
oxygen on the palladium surface. The surface reactions leading to the formation of
hydrogen peroxide and water were assumed to be rate determining, and the rate equations
describing direct synthesis, water formation as well as peroxide hydrogenation and
decomposition were derived. A special kind of product distribution analysis was used to
interpret the kinetic phenomena and to make the estimation of the kinetic parameters very
robust. The parameters were estimated by nonlinear regression analysis and the model
gave a good fit to the experimental data. The usefulness of the product distribution
analysis was clearly demonstrated. The significance of the batch reactor is it improve in
agitator blade and baffle design, mixing in large batch reactors is ultimately constrained
by the amount of energy that can be applied

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

6.0

Ethyl Acetate

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REFERENCES
1. Batch Reactor. (2005) Wikipedia. [Online]. [Accessed 19th April, 2016]. Available from
World Wide Web: https://en.wikipedia.org/wiki/Batch_reactor
2. Reaction Rate Constant. (2005) Wikipedia. [Online]. [Accessed 16th April, 2016].
Available from World Wide Web: https://en.wikipedia.org/wiki/Reaction_rate_constant
3. Batch and Semi-Batch Reactors. (2015) Science Direct. [Online]. [Accessed 15th April,
2016]. Available from World Wide Web:
http://www.sciencedirect.com/science/article/pii/B9780128013052000023
4. Tapio S., Nicola G., Pierdomenico B., and Juan G.S., Product Distribution Analysis of
the Hydrogen Peroxide Direct Synthesis in an Isothermal Batch Reactor, Elsevier, New
York , 2015, vol. 248.
5. Herbert D.C. and Maohong F., Rate Constant Calculation for Thermal Reactions
Methods and Applications, John Wiley and Sons, New York, 2011, p8.

7.0

APPENDICES

a. CA0 Of Sodium Hydroxide (NaOH)

CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

M1V1= M2V2
(0.1 mol/ L) (200mL) = (M2) (400mL)
M2= 0.05 mol/L
CA0= 0.05mol/L

NaOH concentration in 20 mL sample from the reactor

20 Y
0.1

mol / mL
1000
20
=

Let Y = Amount of NaOH titred (ml)

Conversion,X

X= CNaOH(t=0) - CNaOH(t) x 100%

CNaOH(t=0)

Ethyl Acetate

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CKB 20104-Reaction Engineering

Experiment 1a: The Batch Saponification of

Ethyl Acetate

t1/2= Time when the concentration of NaOH is half converted

Half of NaOH converted= 0.05 mol/L 2
= 0.025 mol/L
Based on the graph:
y = -0.0038X + 0.0493
0.025 = -0.0038X + 0.0493
X = 6.39 min

k= 1/ t1/2 . CA0
= 1/ (6.39 0.05)
= 3.13

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