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 OBJECTIVES:

To measure the rate of saponification reaction (K) between NaOH and


ethyl acetate, using a batch reactor, as a function of temperature and
establish the rate law.

 INTRODUCTION:

Reaction rate, the speed at which a chemical reaction proceeds. It is


often expressed in terms of either the concentration (amount per
unit volume) of a product that is formed in a unit of time or the
concentration of a reactant that is consumed in a unit of time.
Alternatively, it may be defined in terms of the amounts of the
reactants consumed or products formed in a unit of time.

In chemical kinetics a reaction rate constant or reaction rate


coefficient, k, quantifies the rate of a chemical reaction.
For a reaction between reactants A and B to form product C

aA+bB→cC
the reaction rate is often found to have the form:

rA = -d[A]/dt = k[A]n[B]m

Here k(T) is the reaction rate constant that depends on temperature.


[A] and [B] are the molar concentrations of substances A and B
in moles per unit volume of solution, assuming the reaction is taking
place throughout the volume of the solution. (For a reaction taking
place at a boundary one would use instead moles of A or B per unit
area).
The exponents m and n are called partial orders of reaction and
are not generally equal to the stoichiometric coefficients a and b.
Instead they depend on the reaction mechanism and can be
determined experimentally.

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In this experiment we will be determining the rate of reaction
constant of the Saponification reaction

Saponification:

Saponification is a chemical process that converts esters into


alcohols and carboxylic acid salts, the primary component in soaps.
In industrial settings, saponification is predominantly used to
“produce glycerol and soaps from triglycerides by reacting them with
a strong alkali salt such as sodium hydroxide (NaOH)”.
Often times, potassium hydroxide is used in place of sodium
hydroxide to produce more water-soluble soaps, such as those used
in shaving cream.

Additionally, saponification is often used to study reaction kinetics in


the laboratory. For example, the saponification of ethyl acetate
(EtAc) with sodium hydroxide is commonly studied because the
reactants are cheap and non-hazardous, and the reaction can be
easily monitored by measuring the conductivity of the reaction
mixture [1]. In this saponification reaction, ethyl acetate and sodium
hydroxide react to form ethanol and sodium acetate.

CH3CO2C2H5 + Na+ OH- ⇔ C2H5OH + Na+ CH3CO2-

(ethyl acetate) + (sodium hydroxide) ⇔ (ethanol) + (sodium acetate)

Sodium hydroxide and sodium acetate are both strongly ionic, so


they dissociate into their respective ions in a polar solvent such as
water. Since conductivity is a function of ion concentration, the
reaction rate can be calculated from observing the change in
conductivity over time.

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Mechanism:

1) Nucleophilic attack by hydroxide

2) Leaving group removal

3) Deprotonation

This experiment is carried out using a Batch Reactor

Batch Reactor:

The batch 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

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distillation, crystallization, liquid/liquid extraction and
polymerization. In some cases, they are not referred to as reactors
but have a name which reflects the role they perform (such as
crystallizer, or bioreactor).

Figure(1-1) Schematics of a Batch Reactor

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


heating/cooling system. These vessels may vary in size from less than
1 liter to more than 15,000 liters. They are usually fabricated in steel,
stainless steel, glass-lined steel, glass or exotic alloy. 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 usually discharged out of the bottom.

Advantages:
1. High conversion per unit volume for one pass
2. Flexibility of operation-same reactor can produce one product one
time and a different product the next
3.Easy to clean

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Disadvantages:
1. High operating cost.
2. Variable product quality in comparison to a continuous operation.

 THEORY:
Chemical kinetics deal with rates and mechanisms of chemical
reaction without the disguising influence of energy and mass
transfer.
It quantitatively describes the course of reaction with time as a
function of reaction conditions (concentration, pressure,
temperature)
Unfortunately, in most cases the status of current research
does not enable us to predict the elementary steps (reaction
mechanism) of particular reaction a priori. Consequently,
kinetic analyses almost always require experiment.
Reaction rates must frequently be represented by means of
simplified models which do not exactly correspond to the
chemical processes taking place, based on the fit between
model and experiment the kinetic should decide whether the
simplifications involved are truly permissible.

Since we are using equal quantities of A and B, the reaction


then is second order
rA = -d[A]/dt = k[A]2

𝑑𝐶𝐴
-𝑟𝐴 = =K𝐶𝐴 2
𝑑𝑡

𝑑𝐶𝐴
=K𝐶𝐴 2
𝑑𝑡

Rearranging we get:
𝑑𝐶𝑖
=Kdt-
𝐶𝐴 2

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Taking integral:
𝐶
𝑡
𝑑𝐶𝑖
∫ = 𝑘 ∫ 𝑑𝑡
𝐶𝐴 2 0
𝐶𝐴0

−2
∫ 𝐶𝐴 𝑑𝐶𝐴 = Kt

Finally, we get:
1 1
= Kt +
𝐶𝐴0 𝐶𝐴

 EQUIPMENT:

Figure(2) stirred tank reaction in series

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-Tools:

1. 250ml glass flask.


2. 500ml glass beaker.
3. Stopwatch.
4. Stirrer.
5. Scale.
6. Stirred Tank Reactor in Series device (as in figure 1)

-Chemical Substances:

1. Sodium hydroxide ( NaOH ).

2. Ethyl acetate ( CH3 COOC2 H5 ).

3. Distilled water.

 Procedure:

Experiment A
Getting the (Conductivity vs Concentration) Calibration
1. Prepare different concentrations of sodium hydroxide (0.005 ,
0.02 ,0.03 , 0.04 , 0.05)M

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2. Measure thermal conductivity by using conductivity meter for
each concentration.
3. Plot CA(x) against K(y) and get an equation that represents the
relationship between the two parameters.

Experiment B
1. Prepare two solutions of NAOH and ethyl acetate by the same
quantity and concentration (0.05 M).
2. Put the solutions in the reactor at the same time and turn on the
stirrer.
3. Start the stop watch.
4. Record the conductivity every 5 minutes for 40 minutes.
5. Plot 1/CA(y) against t(x).

 RESULTS AND CALCULATIONS:

Experiment A

Results:

Concentration (M) Conductivity (µS)


0.005 1.18
0.02 3.85
0.03 6.12
0.04 8.31
0.05 10.32

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Graph:

Concentration vs Conductivity
4.5
4
3.5
3
Conductivity

2.5
2
1.5
1
0.5
0
0 5 10 y15= -0.0892x + 3.542 20 25
Concentration R² = 0.8898

We accuried the equation that represents the relationship between K and CA


K=205.97CA – 0.017

Experiment B
Preparing a 0.05M solution for each of NaoH and ethyl acetate:
NaOH:
W = Mwt*V*M
MWT = 40 g/gmol
V = 0.5 L
M = 0.05
W = 40 * 0.5 * 0.05 = 0.5 g
Ethyl acetate:
Mwt = 88 g/gmol
V = 0.5
M = 0.05
W = 88 * 0.5 * 0.05 = 1.1 g

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Results:

Time (min) K(mS) CA (using Equation) 1/CA


0 3.84 0.018726 53.40161
5 2.88 0.014065 71.09769
10 2.41 0.011783 84.86609
15 2.14 0.010472 95.48911
20 1.98 0.009696 103.1397
25 1.86 0.009113 109.7336
30 1.78 0.008725 114.6188
35 1.72 0.008433 118.578
40 1.67 0.008191 122.0925

Graph:

1/CA vs Time
140

120

100

80 y = 1.6365x + 64.272
1/CA

R² = 0.9285
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40 Slope = K

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0
0 5 10 15 20 25 30 35 40 45
Time

-Slope = 𝐾 = 1.636515
*Using the equation from the first graph we can calculate the corresponding value of CA
-K=205.97CA – 0.017 1.636515=205.97CA – 0.017 CA= 0.008028
-Intercept = 1/CA0 = 64.27161
CA0−CAF 0.0187−0.00819
-Conversion XA = * 100 = * 100 = 56.2%
CA0 0.0187

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 CONCLUSION:
From the results and graphs obtained from experiment A we
conclude that the relation between (K) and (CA) is directly
proportional, higher concentrations give us higher conductivity rates.

Also; from experiment B, we conclude that the conductivity gradually


decreases in time due to the decrease of concentration of the
chemical substances that are being used in the Saponification
reaction.

 DISCUSSION AND SUMMARY:


In summary, the reaction between ethyl acetate and sodium hydroxide
to form sodium acetate and ethanol (Saponification Reaction) was
studied using a batch reactor, the experiment was carried out in room
temperature using a Continuous Stirred Tank Reactor in Series Armfield
equipment after detaching one of the reactors and using it alone a single
Batch Reactor.
Using a concentration of 0.05M for both chemical substances, and
carrying the reaction out in room temperature gave us a Chemical
Reaction Rate (K) of 1.636515 and a conversion of 56.2%

 RECOMMENDATIONS:
There were few recommendations in order to overcome the possible
errors. Firstly, the chemical preparation of the solution of NaOH and
Ethyl Acetate should be done carefully so that no disrupted results can
occur. Secondly, the Batch must be cleaned before and after the
usage to prevent contaminations.
Due to time limitations and scarce resources, Experiment A results were
taken directly from the lab manual , also Experiment B were not given
enough time to reach a steady-state.

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 REFERENCES

1. Octave Levenspiel , Chemical Reaction Engineering , Oregon State


University.

2. Internet Website: www.armfield.co.uk

3. Batch Reactor. (2015) [Wikipedia]:


www.wikipedia.org/wiki/Batch_reactor

4. Smith ,J.M, Chemical Engineering Kinetics , McGraw Hill , 1981.

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