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1.

0 SUMMARY
Ester saponification process is a reaction between ethyl acetate and sodium hydroxide
solution. This experiment is conducted to determine the rate constant for the reaction.
For the first step, the ethyl acetate was reacting with the strong base which was sodium
hydroxide solution to yield carboxylate ion. However, this reaction is relatively slow. Then,
this mixture separated to six different conical flasks that contain hydrochloric acid (HCL) at
different time. Therefore, titration can be done by the reaction of excess HCL and sodium
hydroxide for neutralization. Phenolphthalein was used as an indicator for this reaction. The
volume of sodium hydroxide solution used to change the colourless solution is recorded for
different of time and used to plot graphs and value of concentration of ethyl acetate also can
be calculated. Finally, we can find the reaction rate constant by using integrated law method
and half-life method.

2.0 AIM
The aim for this experiment is to measure the rate constant of the reaction between ethyl
acetate and sodium hydroxide under batch conditions.

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3.0 INTRODUCTION
There are two types of reaction in chemical engineering process which are batch process and
continuous process. In a batch process, input materials are placed in a vessel or reactor, and
the product is withdrawn after the reaction or when the process is complete. This is common
steps of what is usually done in chemistry laboratories. In a steady-flow continuous process,
there is a continuous flow material in and a continuous flow of material out. No separate
filling and emptying operation are required.
Saponification is a process that produces soap from fats and lye. For this experiment,
saponification process in a batch condition, where the reaction between an ester( ethyl
acetate) and sodium hydroxide would be experimented and studied. Theoretically,
saponification involves base (NaOH) hydrolysis of triglycerides, which are esters of fatty
acids, to form the sodium salt of carboxylate.
Saponification is an exothermic chemical reaction which occurs when fats react with the
alkaline solution. So, the reaction will exerts heat to the surrounding. In addition, there is no
heat transfer channelled into the system, meanwhile the mixture stirred continuously. The fats
are being hydrolysed into three fatty acids, which then paired up with the alkali to form crude
soap.
+ C2 H 5 OH
CH 3 COOC 2 H 5+ OH CH 3 COO

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4.0 THEORY

4.1 Second Order Reaction and Reaction Rate Constant


By definition, Second Order Reaction is symbolized by the property where the rate is directly
proportional to the product of two different reactants concentrations or the square of one
reactant concentration
A Product

Rate=k [ A ]

(1)

OR
A + B Product

Rate=k [ A ] [B]

(2)

The coefficient k is called the rate constant for the reaction (Atkins & Paula, 2006). The rate
constant is independent of the concentrations but depends on the temperature. For a chemical
reaction where substance A and B are reacting to produce C, the reaction rate has the form;
Reaction A + B = C

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d [C ]
=k ( T ) [ A ]m [B ]n
dt

(3)

where,
k (T) is the rate reaction constant that depends on temperature.
[C] is the concentration of substance C in moles per volume of solution assuming the
reaction is taking place throughout the volume of the solution.
The exponents m and n are called orders and depends on the reaction mechanism.
They can be determined experimentally.

4.2 Analysis Procedure


In order to monitor the reaction of the experiment conducted, it is important to identify and
measure the amount of unreacted NaOH at suitable time intervals. It is because the
concentration of NaOH is equal with the concentration of ethyl acetate solution. Meanwhile,
the reaction mixture can be monitored by using titration method. In titration method, a small
volume of sample is pipetted from the reaction vessel and purged in a known volume and
concentration of HCl. The excess HCl will titrate NaOH. From this titration the amount of
unreacted NaOH can be determined and used in the determination of the rate constant, k. A
proper technique of pipetting and titration will produce more quality results.

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4.3 Integrated Rate Law Method


For this process, the following assumptions were made to simplify analysis; the process is
irreversible, second-order process and the concentration of ester and hydroxide are equal at
c
the start of the experiment ( )

Thus, the following rate law can be formed:

OH
d [ ester ]
Rate=
=k [ ester ]
dt

As the initial concentration is denoted as

, thus the concentration after time

is

denoted as c .

OH

dc
=k [ ester ]
dt

(4)

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Consequently, the variables are separated and integrated with appropriate boundary
conditions:
1 1
=kt
c c

Therefore, as shown above, by plotting

(5)

1
c

against t, a straight line of gradient k can be

obtained ( Brady, Jespersen & Hyslop, 2012).

4.4 Half-life Method


From equation 5, we can rearrange it to give us :
1 c c
k=
t c c
(6)

Let

k=

t 1 /2

be the time taken for the concentration of ester to be halved, Thus :

1
t 1/ 2 c

From the above relation, we can see that the time taken to halve the concentration of ester is
inversely proportional to the initial concentration (Brady et al., 2012) Therefore, by plotting a

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graph of the concentration of ester

determine

t 1 /2

(c )

against time, it is theoretically possible to

and consequently the rate constant.

6.0 EXPERIMENTAL PROCEDURE


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250 cm

of 0.1 M

ethyl acetate solution was pipetted and transferred into a clean dry

conical flask. 250 cm

beaker. Then, 25 cm

of 0.1 M

sodium hydroxide solution was added into a large

of 0.1 M HCl is pipetted into six different clean labelled 1 - 6

conical flasks. A mechanical stirrer was then placed into the sodium hydroxide, NaOH
solution. The ethyl acetate in the conical flask was then poured into the beaker when the
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mechanical stirrer was turning on. The stopwatch was set to start at roughly the mid-point of
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addition. After 5 minutes, 25 cm

of the reacting mixture was withdrawn by using a

pipette. The solution was then added into conical flask 1. The temperature of the mixture in
the beaker was recorded at the same time when the solution was being pipetted from it. Then,
several drops of phenolphthalein were added in the conical flask 1 as an indicator. The
content of conical flask 1 was then titrated against 0.1 M

sodium hydroxide. The volume

of sodium hydroxide titrated until the moment when the colourless solution changed to pink
was recorded. Several more samples were withdrawn at the following interval; 10, 20, 30, 50,
and 75 minutes, and the procedures were repeated.

6.1 Determining ester concentration, c


Throughout the chemical reaction, the sodium hydroxide are continuously used up in the
reaction with ester.A small sample of the mixture are pipetted into a conical flask filled with
acid, so the sodium hydroxide presents immediately reacted with acid, hence, the reaction
between sodium hydroxide are ceased to occur. The remaining acid are titrated against
sodium hydroxide. This allowed us to relate to sodium hydroxide and ester in the original
sample.

The volume of 1 litre of NaOH is denoted as

y cm3 .

The number of 0.1M NaOH used in titration is expressed as;


0.1 y
=acid neutralised titration
1000 mol

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The original quantity of 0.1M acid is;


0.1 25
=0.0025
1000

Thus, the acid neutralised by sample can be related as;


0.1 ( 25 y )
=moles of NaOH present t h e sample
1000

Hence, the concentration of NaOH in

25 cm 3

sample from the reactor is equal to the

concentration of ester (c) when :

( 25 y )
mol
0.1
25
x
(7)
1000
cm 3

6.2 Determining Reaction Constant , k in Second Order Reaction


The reaction of saponification of ethyl acetate is relatively a slow process. Thus, the change
in concentration of ester can be followed by simply analysing the samples from the reacting
mixtures at different time intervals. The rate constant for second order of reaction can be
determined in two different methods, which are integrated law method and half-life method.

7.0 EXPERIMENTAL RESULTS

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The table below shows the correlation between time(t) of reaction occurring to
the volume of sodium hydroxide that was determined via titration.

Table 1.0 : Tabulation of results from ecperiment conducted


Flask

Time (min)

Volume of

Mole of

Concentration

NaOH (ml)

NaOH

ester ( c)

present in the

mol /dm

1
c

dm 3 /mol )

22

sample (mol)
4
3 10

10

22.5

2.5 104

20

23.7

1.3 10

30

24.0

1 104

4.0 103

250.00

60

24.0

1 104

4.0 103

250.00

75

24.2

8 105

3.2 103

312.50

12 10

83.33

10 103

100.00

5.2 10

192.3077

The volume of sodium hydroxide used is then used to determine the concentration of ethyl
acetate, (c).The concentration of ethyl acetate, (c) can be calculated using equation number

(7).For first method, the integrated rate law method, the value

1
c

is plotted against time to

determine the value of rate constant (k).For second method, the half-life method, the value
(c) is plotted against time to determine the value of rate constant (k).

8.0 ANALYSIS AND DISCUSSION


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8.1 Integrated Rate Law Method

1/c against time, t


350

f(x) = 3.13x + 98.76

300
250
1/c, dm3 200
/mol2
150
100
50
0
0

10

20

30

40

50

60

70

80

Time, t (min)

Figure 1.2: The graph above shows the relationship between

1
c

and time (t).

From the graph above, the following graph equation (software generated) is fomed ;
y = 3.1347x + 98.757

(8)

Provided that, the gradient of the slope is equal to k. Hence we can conclude that;
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k=

3.134 d m 1 min
x
=0.0522 d m3 /mol s
mol . min
60 s

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8.2 Half- life method

concentration of ester,c against time,t


0.01
0.01
0.01
concentration of ester, c, mol/dm3

0.01
f(x) = 0.01 exp( -0.02 x )
0.01
0
0
0
0 10 20 30 40 50 60 70 80

time, t (min)

Figure 1.3 : The graph above shows the relationship between the concentrations of ethyl
acetate to the time of reaction.
To calculate the exact value of t1/2, use the function of the graph (software generated), ;
y = 0.0098e-0.018x
let y = 0.00506 , then,
0.00506 = 0.0098e-0.018x
0.516 = e-0.018x
-0.018x = -0.661
Therefore x= 36.69 minutes

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Equation number (6) is used to calculate the value of rate constant, k with initial
concentration of ethyl acetate (c0) is equal to 0.0101 mol/dm3. Based on previous calculation,
the time required to achieve half of co (0.00506 mol/dm3) is 36.72 minutes.
Hence;

k=

Based on the graph

1
1
1 min
3
=
x
=0.0445 dm /mol s
t 1/ 2 c ( 36.69)(0.0101) 60 s

1
c

against time, the value of k is 0.0522 d m /mol s while from

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graph c against time , the value of k is 0.0445 dm /mol s . This difference of value maybe

was caused by some errors during the experiment was conducted such as parallax error. This
kind of error occured when taking the reading from apparatus where the meniscus level of
formed from solution is not read accurately. In order to prevent this error, students should
locate their eyes parallel to the level reading of apparatus.

9.0 CONCLUSION
The experimental value of rate constant in a reaction between ethyl acetate and sodium

hydroxide under batch condition is

0.0522 d m /mol s

when the value is determined by

using integrated rate law method. On the other hand, the rate constant that was determined
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by using half-life method is 0.0445 d m /mol s .

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10.0 REFERENCE
Atkins, P., & Paula, J. de (2005). Physical Chemistry (8th ed.). New York; W.H. Freeman and
Company
Brady, J. E., Jespersen, N. D., & Hyslop, A. (2012). Chemistry. John Wiley and Sons, Inc.
http://chemwiki.ucdavis.edu/Physical_Chemistry/Kinetics/Reaction_Rates/Second_Order_Re
actions [28 June 2013, 11.34 PM]

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