DETERMINATION OF RATE CONSTANT FOR SPONIFICATION OF

ETHYL ACETATE WITH NaOH VIA CONDUCTIVITY IN BATCH

REACTOR FOLLOWED BY INTEGRAL ANALYSIS

1. ABSTRACT:
In this experiment we are trying to find the rate constant of saponification reaction in
batch reactor by integral analysis. For this purpose we made 1000 ml solution of NaOH
and ethyl acetate of 0.06 M. put their half amounts an a batch reactor and find their
temperature and conductivity at every 1 minute interval. After this draw the graph
between the inverse of CA and temperature. The slope of the graph gives rate constant.
The saponification reaction gives second order rate equation.

2. APPRATUS:
 Glass wares (beakers)

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 Batch reactor (CEB-MKll) mounted on chemical reactor service unit (CEX-Mll)

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 Glass Thermometer

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 Conductivity Meter

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3. REAGENTS:
 Distilled water rs e
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 1 liter standard NaOH solution (0.06 M)
 1 liter standard Ethyl acetate solution (0.06 M)
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4. INTODUCTION:
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Saponification is a process by which triglycerides are reacted with sodium or potassium

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hydroxide to produce glycerol and a fatty acid salt, called "soap." The triglycerides are
most often animal fats or vegetable oils. When sodium hydroxide is used, a hard soap is
produced. Using potassium hydroxide results in a soft soap. Example of saponification
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reaction is reaction between ethyl acetate and NaOH (1).

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In this experiment the saponification reaction occurs in Batch Reactor. The batch
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reactor is the generic term for a type of vessel widely used in the process industries. Its
name is something of a misnomer since vessels of this type are used for a variety of
process operations such as solids dissolution, product mixing, chemical reactions, batch
distillation, crystallization, liquid/liquid extraction and polymerization. A batch reactor
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may be described as a vessel in which any chemicals are placed to react. Batch reactors
are normally used in studying the kinetics of chemical reactions, where the variation of a
property of the reaction mixture is observed as the reaction progresses. Data collected
usually consist of changes in variables such as concentration of a component, total
volume of the system or a physical property like electrical conductivity. The data

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 collected are then analyzed using pertinent equations to find desired kinetic parameters
(2).

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Fig: 1 (Batch Reactor)

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A typical batch reactor consists of a tank with an agitator and integral heating/cooling

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system. Liquids and solids are usually charged via connections in the top cover of the
reactor. Vapors and gases also discharge through connections in the top. Liquids are

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usually discharged out of the bottom. The advantages of the batch reactor lie with its
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versatility. A single vessel can carry out a sequence of different operations without the
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need to break containment. This is particularly useful when processing toxic or
highly potent compounds (3).
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aC s
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Fig: 2 (Schematic diagram of batch reactor)

The equations we get from the experimental data of saponification of ethyl acetate and
NaOH in batch reactor are:
(1)
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 λ AO =λO =0.195[1+0.0184(T −273)C AO ]

λC ∞ =λ∞ =0.070 [ 1+0.0284 ( T −273 ) CC ∞ ] (2)

λo − λ
C A =( C A ∞ −C AO ) +C Ao
λ0 −λ∞ (3)

λ AO λC ∞
In equation (1)and (2) and are the initial and final conductivity of the
C AO CA ∞
component. In equation (3) and are the initial and final concentration of
the component.

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Initial concentration of NaOH in reactor = CAO = 0.06 / 2 = 0.03 M

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Concentration of NaOH after infinite time = CA∞ = CAO – CBO = 0

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Concentration of Na- acetate in reactor after infinite time = CC∞ = CAO = 0.03 M
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Initial conductivity of solution in reactor at zero time = λo = λAo + λco = λAo ( λco = 0)

5. SOLUTION PREPERATION:
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Ethyl acetate solution:

To prepare 0.06 M solution of ethyl acetate we have to find its volume so,
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mass=moles × molar mass

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mass=0.06 ×88
mass=5.28
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mass
volume=
density
5.28
volume=
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0.898
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volume=5.87 ml

So, we will add 5.87 ml of ethyl acetate in 995 ml of water.

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NaOH SOLUTION:
We have to prepare 0.06M solution of NaOH. For this purpose we have to find how much
grams of NaOH is needed .to pre pare the solution we need 1L of distilled water.
No . of moles of NaOH
M=
1 dm 3 of solution

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 mass
molar mass
0.06=
0.25

mass
40
0.06=
1
mass=2.4 g

To prepare the solution add 2.4g of NaOH in a beaker and add distilled water up to 1L to
make 0.06M solution of NaOH.

6. EXPERIMENTAL WORK:

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 First prepare 1000 ml standard solution of NaOH and ethyl acetate of 0.06 M.

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 Measure their temperature and conductivity at zero time in reaction vessel.

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Add 500 ml of NaOH and ethyl acetate in a batch reactor and start stirring.

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
 Measure temperature and conductivity at every 1 minute interval.

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 Take the reading until the steady state (no change in conductivity) is achieved.
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After that make the graph between inverse of CA and temperature.
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 The slope of the graph gives rate constant K.

7. RESULT AND CALCULATION:

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There are three types of reaction can occur in saponification reaction in which:
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 CA=CB
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 CA<CB
 CA>CB
For the first case in which concentration of component A is equal to component B the rate
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equation is:
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−r A=k C A C B
2
−r A=k C A
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−d C A
=k C2A
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dt
After integrating the equation we get:
1 1
− =kt
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C A C Ao

1 1
=kt+
CA C Ao

By comparing the equation with y = mx + c we get:

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 1
 y= CA

 m=k
1
 c= C Ao

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λ(mS ) Time T λo ( S) λ∞ (S) λo − λ 1

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(min) (○C) C A =( C A ∞ −C AO ) +C Ao (-
λ0 −λ∞ CA

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1
M)

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5.8 0 17 0.00767 0.00311 0.017 58.8
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9
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4.8 1 17 0.00767 0.00311 0.030 33.33
9
4.6 2 17 0.00767 0.00311 0.0098 102
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9
aC s

4.3 3 17.5 0.00773 0.00314 0.0075 133

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3
4 4 17.5 0.00773 0.00314 0.005617 178
3
4 5 17.5 0.00773 0.00314 0.005617 178
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3
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4.3 6 17.5 0.00773 0.00314 0.0075 133

3
4.3 7 17.5 0.00773 0.00314 0.0075 133
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3
4 8 17.5 0.00773 0.00314 0.005617 178
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3
4 9 17.5 0.00773 0.00314 0.005617 178
3
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Table: 1

Graph:

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 (-1M)
200
180 f(x) = 13.58x + 69.41
160
140
120 (-1M) Linear ( (-1M) )
100
80
60
40
20
0
0 1 2 3 4 5 6 7 8 9 10

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Fig: 3 (Time VS Inverse of Concentration)

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From the graph the value of slope is 13.579 and y-intercept is 69.409.

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8. CONCLUSION:
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In this experiment we have to find the rate constant for the rate equation. The graph
between time and inverse of concentration gives us the slope which is equal to the rate
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constant of the equation. A very small value for the rate constant equates to a very slow
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reaction in general. Equally, a large value for the rate constant means a large value for the
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rate and that the reaction is rapid. Time and concentration have inverse relation, as the
time increases concentration decreases. But concentration and conductivity have direct
relation, as the increase in concentration conductivity increases.
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9. REFRENCES:
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1) https://www.thoughtco.com/definition-of-saponification-605959
2) http://khartoumspace.uofk.edu/bitstream/handle/123456789/10162/Saponific
ation%20A%20Comparative%20Kinetic.pdf?sequence=1&isAllowed=y
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3) https://www.cambridge.org/core/books/mathematical-modeling-in-chemical-
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engineering/empirical-model-building/6EDF77DAD71636EE7AE0B3333BF6
4) Lab manual
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