UNIVERSITY OF SABRATHA

FACULTY OF ENGINEERING DEPARTMENT OF CHEMICAL ENGINEERING

UNIT OPERATION 2 CHE 432

EXP3
determine the rate constant of saponification reaction by using batch reactor

Prepared By

Students Name Sign

-1 ‫مرام الطاهر محمد أبوالقاسم‬

-2 ‫آالء محمد الهادي القمودي‬

Under the supervision of

Mr. Nader Kmal

Date of experimental 02/06/2022

Objectives:

To determine the reaction rate constant (k) for the given sponification reaction of
ethyl acetate in aqueous sodium hydroxide solution in a isothermal batch reactor.

Introduction:

In this reaction, the saponification reaction between sodium hydroxide (NaOH) and
ethyl acetate (EtAc) was conducted. The reaction was conducted using equimolar
amounts of both reactants to produce ethanol (EtOH) and sodium acetate (NaAc). In
addition to, the kinetic parameters for the reaction were determined. To determine
the concentration of NaOH in the reaction and to monitor reaction progress,
conductivity was measured; hence, conductivity can then be turned
into concentration using calibration curves of the products and the reactants. After
the concentration vs time graphs are generated.

Theory
The Armfield batch reactor is designed to demonstrate the mechanism of a chemical
reaction in a reactor, as well as the effects of varying process conditions such as
reaction temperature and reagents concentrations. In this experiment, the
Saponification of Ethyl acetate by Sodium hydroxide is the reaction chosen to study
these conditions

NaOH + CH3COOC2H5 → CH3COONa+ C2H5OH

For this second order elementary reaction the rate equation is:

−r A =k . C A .C B (1)
Where:
rA = rate of reaction (mol.L-1.S-1)
K = reaction rate constant (S-1)
CA = concentration of NaOH (mol.L-1)
CB = concentration of Ethyl acetate (mol.L-1)

If the initial concentrations of reactants are equal, then

−d C A 2
=k .C A ( 2 )
dt

Integration of this rate law for a single reactant gives:

1 1
=k .t + (3)
CA CA 0
t = time (s)
C A 0= initial concentration of NaOH (mol.L-1)

Hence, a plot of 1/C A against t gives a straight line of gradient k and an intercept of
1/C A 0
The relationship between the concentration and conductivity is:

C At=( C A ∞ – C Ao )
( Λ0 − Λt
Λ0 − Λ∞ )
+C Ao ( 4 )

Where

𝛬𝑜 = initial conductivity (Siemens/cm)

𝛬∞ = conductivity after ∞ time (Siemens/cm)
𝛬 = conductivity at time t (Siemens/cm)
concentration of NaOH after ∞ time (mol.L-1) = C A ∞
.Once CA is determined, then by using equation (3),K can calculated

Description of the equipment :

 The concentration will be monitored throughout the reaction time by measuring

the electrical conductivity through a conductivity sensor supported inside the
reactor. An electrical digital water bath will be used to heat the reactants initially
and prior to mixing them into the reactor tank.
 the conductivity is displayed on units of millisimens/cm. During the chemical
reaction, the conductivity of the reacting solution changes as more of the
reactants are converted. This data can be logged and used to determine the
degree of conversion and the rate of reaction.
 Figure1- Batch reactor

Experimental procedure

1. Solution Preparation

Dilution of Sodium hydroxide :

 Take 5 g of sodium hydroxide (Mw = 40 g/mol) to prepare 250Ml of sodium
hydroxide 0.5 M.
m 5
C= = =0.5 mol/ L
Mw ×V 40 × 0.25

Dilution of ethyl acetate :

 Take 12.36Cm3 of ethyl acetate ( ρ = 0.89 g/cm3 , Mw = 88.11 g/mol) to prepare
11g , 250Ml of ethyl acetate 0.5 M.

m=Mw × V ×C
m=88.11 × 0.25× 0.5=11 g
m m
ρ= → V =
V ρ
11 3
V= =12.36 cm
0.89

2. Ensure that the conductivity sensors has been installed correctly.

3. Charge the batch reactor with the 0.25 liter of sodium hydroxide solution. Set the
reactor agitator to 100% and press 'power on' to start the agitation.
4. Carefully add to the reactor 0.25 liters of ethyl acetate solution. Conductivity with
respect to time will be collected for about 20 minutes as chosen previously.
5. Start the stopwatch and write the value of the Conductivity from the mentor every
minute.

Raw data:
Table1.raw data
t (min) Λ (mSiemens /cm)
2 18.5
3 17.22
4 16.45
5 16
6 15.66
 7 15.40
8 15.21
9 15.07
10 14.94
11 14.86
12 14.78
13 14.71
14 14.65
15 14.61
16 14.56
17 14.52
18 14.50
19 14.48
20 14.45
Calculations:

To calculate Λ a 0 :

Λ a 0=0.195(1+0.0184 (T −294)) a0

Room temperature: T =27+273.15=300.15 K

Λ a 0=0.195 ( 1+0.0184 ( 300.15−294 ) ) ×0.5

Λ a 0=0 .1085 Siemens

Λ a 0=108.5 mSiemens

C At=( C A ∞ – C Ao )
( Λ0 − Λt
Λ0 − Λ∞)+C Ao

C Ao=0.5 mol / L C A ∞=0

Λ a 0=108.5 mSiemens/cm Λ ∞=14.45 mSiemens/cm

Table2. calculations
t (min) Λ (mSiemens /cm) C At 1/ C At
0 108.5 0.5 2
2 18.5 0.0215 46.51
3 17.22 0.0147 68.03
4 16.45 0.0106 94.34
5 16 0.0824 121.359
6 15.66 0.0064 156.25
7 15.40 0.00505 198.02
8 15.21 0.00404 247.52
9 15.07 0.003296 303.398
10 14.94 0.0026 384.62
 11 14.86 0.00218 458.72
12 14.78 0.001754 570.13
13 14.71 0.00138 724.64
14 14.65 0.001063 940.73
15 14.61 0.000851 1175.09
16 14.56 0.000585 1709.4
17 14.52 0.000372 2688.17
18 14.50 0.000266 3759.4
19 14.48 0.0001594 6273.53
20 14.45 0 ∞

1
Then plot on Y axis and t on X axis:
CA

1 1
=k .t +
CA CA 0

0007

0006

0005

0004
AC/1

0003

0002

0001

0
0 2 4 6 8 01 21 41 61 81 02
)nim( t

1
VS t -Figure2
CA
:Use Excel to determine the slope

S 213.9609 Slope=K=¿
−1

:Results and Discussion

From the results the concentration of NaOH is decreasing with time, at the end the
concentration becomes zero.
Conclusion

Based on the data and graph plotted, it can be concluded that:

1. Sodium hydroxide reacts with ethyl acetate to form sodium acetate and ethyl
alcohol; as a result, the concentration of sodium hydroxide was reported to
decrease with time.
2. It was noted that the concentration-time curve slope change with time, where the
curve becomes less steep at the final stage, due to the decrease in reagents
concentrations.

Recommendation

There are several precautions and recommendations that we can do to ensure more
accurate and reliable results. Which are:

1. Always make sure that the start-up procedure and shut down procedure was
done correctly to prevent damage at the equipment.
2. Link the conductivity reads and save data continuously with higher accuracy and
precision to save effort and ensure better accuracy.
3. Glass apparatus need to be handled carefully to prevent it from breaking while
experiment
4. The Batch reactor must be cleaned before and after the usage to prevent
contaminations

References:

1. Chemical Engineering Laboratory (4) Manual Sheet Batch Reactor, 2016 ,

University of Jordan Faculty of Engineering and Technology Department of
Chemical Engineering Chemical Engineering
2. https://www.academia.edu/77163367/
Saponification_reaction_of_ethyl_acetate_and_sodium_hydroxide_using_differen
t_reactors
3. Nader nasar, Adli alznati, and Abdulozez Arzoga, the effect of reactants' initial
temperatures on therate constant and conversion of saponification reaction taking
place in a non-isothermal and nonadiabatic batch reactor, Department of Chemical
Engineering, Faculty of Engineering, Sabratha University, Libya