GROUP G1-4

REACTION ENGINEERING
Experiment 4 A: Isothermal Operation
Batch Reactor

Experiment date: 20/03/18

Report Submission date: 28/03/18

Group Members:
Name ID Signature
Jeniffer Daniela Olivos 18172340
Berrios

Saravanan Periasamy 18171305

Panji Aryo Prakoso 18895087

Arnadya Paramitha 18109762

Pudhiastono
Table of Contents
Introduction.....................................................................................................................2
Objectives.......................................................................................................................2
Experimental Setup.......................................................................................................3
Experimental Procedure...............................................................................................4
Data Analysis (Calculation)..........................................................................................5
Results and Discussion................................................................................................9
Conclusion....................................................................................................................12
Reference......................................................................................................................13
Appendix.......................................................................................................................14
Appendix A: Data Logger Results................................................................................................14
Appendix B (Nomenclature).......................................................................................................20

1
Introduction
Most of the reactions carried out in a laboratory are using batch reactors. The
reactants are mixed together and placed in a test-tube, flask or beaker. They are
often heated for the reaction to take place and are then cooled (The Essential
Chemical Indutry-Online, 2013).

Figure 1: Illustrating a Batch Reactor

In this experiment, an Armfield CEB MkIII Batch Reactor was used for the study of
an isothermal operation. The reaction rate constant in this experiment will be
calculated through the chemical reaction between sodium hydroxide and ethyl
acetate.

NaOH + CH3COOC2H5  CH3COONa + C2H5OH

Objectives
The objective of this experiment is to find the reaction rate constant in a stirred batch
reactor. The values recorded will be the initial concentration and conductivity values
which are then used to calculate the final concentration.

2
Experimental Setup
The preparation and the installation of the experiment will be explained in this report.
All of the experiment’s set up is originally comes from Armfield’s CEXC, which
contained the Armfield’s CEB MKIII Transparent Batch Reactor with Hot Water
Circulator attached on the setup and the CEXC software in the computer, which can
be seen on figure 2 as all of the equipment are attached.

Figure 2: Equipment Setup (Aermfield 2013)

Before the process happen, all of the equipment and tools necessary for the batch
reactor is unpacked, assembled and installed. The transparent reactor, CEB MKIII
Batch Reactor, is mounted on top of the blue baseplate with nut locked as well as
the Hot Water Circulator. The both temperature and conductivity sensors and also
the stirrer has to be attached to the CEB MKIII Transparent Batch Reactor Lid, which
the lid has a function as a top cover of the reactor. Then, as can be seen on Figure
1, the plastic hose of the HWC has to be connected to the reactors. The HWC is
filled with water until the surface of the water reached 20 mm from the top. The
software is needed to be installed in the computer and RCD cable is connected to
the computer. The power cable is connected to the power supply due to the
electricity source of the reactor.

3
Experimental Procedure
The procedure of this experiment is explained, which contained of the instruction of
running the equipment and collect the data from the software. Before starting the
reactors, two chemical substances are prepared for this experiment, which are 1500
ml of 0.1M Sodium Hydroxide (NaOH) and 1500 ml of 0.1 Ethyl Acetate
(CH3COOC2H5). The experiment will run at three different temperatures, which are
25, 30 and 35 0C. Using gloves and long sleeves during the experiment is important
towards the safety of handling the hazardous chemical that need to be prepared as
the requirement.

First, prepare 500 ml of both sodium hydroxide and ethyl acetate in different
volumetric flask and heat both of the liquid until the temperature of the substance is
25 0C using a heater that provided in the lab. Make sure the HWC and the stir of the
reactor are functioning properly. Then, Insert the 500 ml of the sodium hydroxide into
the reactor first carefully and closed the lid. Open the software and connect the
computer to the CEXC. Several parameters need to be adjusted in the PID
Controller window, which are setting the mode operation to automatic mode and set
the temperature to 25 0C after turning the HWC on. Set the value of the stirrer up to
50 and the reactor temperature is left until it reached 25 0C. After the data for 250C is
created, turn off the stir and the HWC and fill the reactor with 500 ml of Ethyl
Acetate. Turn everything back on again and record the data.

After all of the data and the graph are obtained, turn off the entire recording, HWC
and reactor stir due to the cleaning of the reactor for following set of temperature.
Unscrew the nuts from the base of the reactor and carefully dispose the mixture
inside of the reactor to the disposal basin on the CEXC. After that, clean and rinse all
of the equipment that contaminated with the mixture such as the inside of the
reactor, the sensor and the stirrer with diluted water. Restart the experiment with the
same procedure but different temperature set, which are 30 and 35 0C, and obtain all
of the data.

4
Data Analysis (Calculation)
The results in the tables below have been recorded for one minute interval. The full
record of the results from the data logger is attached in Appendix A.

Time Temperature a1 c1 Xa Xc (a0-a1)/

(s) (K) (mol/dm3) (mol/dm3) (NaOH) (NaAc) (a0.a1)
0 298 0.02573 -0.00073 -0.02928 -0.02928 -1.1380
60 298 0.02233 0.00267 0.10685 0.10685 4.7850
120 298 0.01973 0.00527 0.21089 0.21089 10.690
180 298 0.01765 0.00735 0.29413 0.29413 16.667
240 298 0.01594 0.00906 0.36251 0.36251 22.745
300 298 0.01453 0.01047 0.41899 0.41899 28.845
360 298 0.01341 0.01159 0.04635 0.04635 34.568
420 298 0.01237 0.01263 0.50520 0.50520 40.840
480 298 0.01155 0.01345 0.53790 0.53790 46.561
540 298 0.01081 0.01419 0.56763 0.56763 52.513
600 298 0.01014 0.01486 0.59438 0.59438 58.615
660 298 0.00962 0.01538 0.61519 0.61519 63.948
720 298 0.00910 0.01590 0.63600 0.63600 69.890
780 298 0.00858 0.01642 0.65681 0.65681 76.554
840 298 0.00821 0.01679 0.67168 0.67168 81.830
900 298 0.00784 0.01716 0.68654 0.68654 87.608
Table 1: Results for T = 250C = 298K

Time Temperatur a1 c1 Xa Xc (a0-a1)/

3 3
(s) e (K) (mol/dm ) (mol/dm ) (NaOH) (NaAc) (a0.a1)
0 305.4 0.02337 0.00016 0.06521 0.06521 2.79036
60 306.0 0.01866 0.00633 0.25324 0.253248 13.5653
120 306.1 0.01557 0.00942 0.37716 0.37716 24.2219
180 306.2 0.01329 0.00117 0.46836 0.46836 35.2401
240 306.3 0.01155 0.01344 0.53778 0.53778 46.5393
300 306.5 0.01004 0.01495 0.59083 0.59803 59.5105

5
360 306.5 0.00897 0.01602 0.64113 0.64113 71.4634
420 306.6 0.00798 0.01701 0.68053 0.68053 85.2106
480 306.6 0.00724 0.00177 0.71014 0.71014 97.9982
540 306.7 0.00660 0.01840 0.73598 0.73598 111.505
600 306.7 0.00599 0.01900 0.76017 0.76017 126.790
660 306.7 0.00552 0.01947 0.77899 0.77899 140.992
720 306.8 0.00501 0.01998 0.79936 0.79936 159.368
780 306.7 0.00465 0.02034 0.81394 0.81394 174.989
840 306.8 0.00427 0.02072 0.82905 0.82890 193.788
900 306.8 0.00400 0.02099 0.83964 0.83964 209.449
960 306.8 0.00374 0.02126 0.85038 0.85038 227.359
1020 306.8 0.00347 0.02152 0.86113 0.86113 248.039
Table 2: Results for T = 300C = 303K

Table 3: Results for T = 350C = 308K

Time Temperature a1 c1 Xa Xc (a0-a1)/
3 3
(s) (K) (mol/dm ) (mol/dm ) (NaOH) (NaAc) (a0.a1)
0 310.2 0.0209 0.00401 0.16048 0.16048 7.64616
60 311.4 0.0162 0.00874 0.34978 0.34978 21.5180
120 312.0 0.0131 0.01189 0.47566 0.47566 36.2863
180 312.5 0.0107 0.01426 0.57504 0.57054 53.1405
240 312.7 0.0089 0.01603 0.64112 0.64112 71.4594
300 312.9 0.0076 0.01737 0.69465 0.69465 90.9976
360 313.2 0.0065 0.01849 0.73943 0.73943 113.510
420 313.2 0.0056 0.01936 0.77454 0.77454 137.413
480 313.4 0.0049 0.02006 0.80250 0.80250 162.534
540 313.5 0.0042 0.02072 0.82894 0.82894 193.840
600 313.6 0.0038 0.02120 0.84784 0.84784 222.879
660 313.7 0.0033 0.02167 0.86670 0.8667 260.067
720 313.8 0.0029 0.02208 0.88302 0.88302 310.950
780 313.9 0.0025 0.02242 0.89683 0.89683 347.705

6
 840 314 0.0022 0.02277 0.91061 0.91061 407.458
900 313.7 0.0020 0.02291 0.91660 0.91660 439.609

The nomenclature for the following calculations in attached in Appendix B

The following calculations are based on data at t=540s for T=25 0C
𝑎𝜇 = 0.05 mol/dm3
𝑎0 = 0.025 mol/dm3
b𝜇 = 0.05 mol/dm3
b0 = 0.025 mol/dm3
T = 298 K
V = 1L
c∞ = 0.025 mol/dm3

To find initial conductivity

Λ0 = Λ𝑎0 = 0.195[1+0.0184(𝑇−294)]0 = 0.195[1+0.0184(298−294)](0.025)
= 5.2338 mS

To find conductivity at steady state

𝑎∞ = (𝑎0−𝑏0) = 0.025 – 0.025 = 0
Λ𝑎∞ = 0
Λ𝑐∞ = 0.070[1+0.0284(𝑇−294)].𝑐∞ = 0.070[1+0.0284(298−294)](0.025)
= 1.9488 mS
Λ∞ = Λ𝑐∞+Λ𝑎∞ = 1.9488 + 0 = 1.9488 mS

To find concentration of a at time t= 540s

𝑎1 = (𝑎∞−𝑎0)[(Λ0−Λ1)/(Λ0−Λ∞)] + 𝑎0 = (0 – 0.025)[(5.2338-3.37)/(5.2338-1.9488)] +
0.025
= 0.01081 mol/dm3

c1 = c∞ [(Λ0−Λ1)/ (Λ0−Λ∞)] = 0.025[(5.2338-3.37)/(5.2338-1.9488)] = 0.01419 mol/dm 3

Xa = (a0 – a1)/a0 = (0.025-0.01081)/0.025 = 0.5676

Xc = c1/c∞ = 0.01419/0.025 = 0.5676

(𝑎0−𝑎1)/(𝑎0.𝑎1) = (0.025 – 0.01081)/(0.025x0.0108) = 52.56

A graph of (𝑎0−𝑎1)/(𝑎0.𝑎1) against time is plotted to find the reaction rate constant, k.

(𝑎0−𝑎1)/(𝑎0.𝑎1) = kt

For T = 250C, from graph 2, k = = 0.1021 s-1

7
 1 0.03

Current NaOH concentration 0.8 0.03

0.6 0.02

Conversion Xa
0.4 0.02
a1(mol/dm3

0.2 0.01

0 0.01
0 50 100 150 200 250

-0.2 0

Time (seconds)

X1(298K) X2(303K) X3(308k) a1(298K) a2(303K) a3(308K)

GRAPHS

Figure 3: The relationship between concentrations of NaOH vs Its conversion over

time
500
f(x) = 2.37 x − 39.17
400 R² = 0.96
a0-a1)/(a0.a1)

300

200 f(x) = 1.2 x − 11.51

R² = 0.99
100
f(x) = 0.51 x − 2.56
R² = 0.99
0
0 50 100 150 200 250
-100
Time(seconds)

298K Linear (298K) 303K

Linear (303K) 308K Linear (308K)

Figure 4: Determination of rate constant, k

When T = 250C, k = 0.1021 s-1

When T = 300C, k = 0.2401 s-1
When T = 350C, k = 0.4738 s-1

8
 0
0.5 1 1.5 2 2.5 3 3.5 4 4.5

-0.5

-1
In K

-1.5

-2

-2.5
1/T (K)

Figure 5: Relationship between reaction rate and temperature

Results and Discussion

The objective of the experiment was to find the reaction rate constant in a stirred
batch reactor. Saponification of ethyl acetate by sodium hydroxide was the reaction
selected under isothermal conditions and the Armfield CEB software allows us to
obtain real-life data of the temperature, conductivity and stirred speed during the
experiment.
Saponification of ethyl acetate by sodium hydroxide is a second order reaction; the
reaction rate constant can be calculated assuming the equimolecular concentrations
of both reactants.
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH

a-X + a-X → X + X
The rates of any chemical reaction depend on temperature and composition of the
reactants. At higher temperatures particles of the reactants move faster creating
collisions. The same behaviour will occur by particles when reactants have a high
concentration. The Arrhenius Equation can measure these two terms.k
−E a/( RT)
k=Ae
Where

 k is the rate constant

9
  T is the absolute temperature (in kelvins)
 A is the pre-exponential factor, a constant for each chemical reaction.
 Ea is the activation energy for the reaction (in the same units as R*T)
 R is the universal gas constant.

Activation energy and rate constant can be calculated by re-arranging the Arrhenius
equation.
Sodium Hydroxide (NaOH) is used as a reference during the calculations due its
limiting role during the reaction and the high conductivity of its ions. The high
conductivity of NaOH was calculated during the data analysis where we can observe
that the initial conductivity (Λ 0 = 5.2338 mS) is higher than the conductivity at steady
state (Λ∞ = 1.9488mS) where only a few ions are present. Therefore, when NaOH
reacts, the conductivity will decrease.
Analysing the data, the relationship between concentrations of NaOH verses
conversion over time were plotted in a graph. It can observed that the concentration
of NaOH decreased with the increase in its conversion over period of time, because
the concentration of NaOH had been consumed.
The saponification reaction can be written as
A + B -> products,
A being NaOH. The rate law can be written as
rA = - kCACB
Combining the above rate law with mole balance on A.
dCA/dt = -kCACB – (v0/V)CA
During the reaction when ethyl acetate is added to sodium hydroxide in the reactor,
both reacted immediately to produce the products, so we can observe the decrease
in the concentration of reactants while the concentration of the products is increased.
In the graph we can observe that the concentration of NaOH decreased with the
increase in temperature. The highest concentration of NaOH is at 25°C. At 30°C,
NaOH concentration lower than 25°C and at 35°C the concentration is lower than
30°C. When the temperature is increased the particles move faster and the
concentration of reactants is consumed faster leading to conversion increases at
greater temperatures.

For the determination of the rate constant, a graph with the relationship between (a0-
a1)/a0.a1 and time is plotted. In the graph we can observe that k depends on the
temperature of the reactor. As temperature is increased, k also increases.

 When T = 250C, y = 0.1021x - 2.0487

R² = 0.9884

10
 k = 0.1021 s -1

 When T = 300C, y = 0.2401x - 10.305

R² = 0.99227
k = 0.2401 s -1

 When T = 350C, y = 0.4738x - 36.8

R² = 0.96436
k = 0.4738 s-1

To understand the relationship between the reaction rate constant as a function of

the temperature, a graph between 1/T on x-axis and lnk on y- axis by using
experimental data.

The results show that

y = -13723x + 43.808

Straight line equation y= mX + c

ln k0= 43.808 k0=10.607 x1018 m3/mol sec

m= (Ea /R)=13727

Ea=13727 x 8.314= 114.13 KJ/mol

Reaction rate constant in function of the temperature

Ln K(T)= 43.808 -13723 (1/T) T=(kelvin)

Experimental errors should be considered. During the data collection when t=0min
the concentration of NaOH is a negative number since the experiment started before
the ethyl acetate was added. Another error was that the reading of the temperature
of the reactor was not working and external thermometers were used. And last, a
possible error may have occurred during the heating of ethyl acetate to the required
temperature due to the multiple thermometer readings because of the malfunction of
the reactor.
In the graph where the relationship between the reaction rates constant in function of
the temperature are showed, we can observe that the result almost fit the linear line.
This means that the data recorder was correct, not highly precise but close enough.

11
Conclusion
The objective of the experiment was to find the reaction rate constant during the
Saponification of ethyl acetate by sodium hydroxide reaction. Armfield CEB software
allows us to obtain the data.
The experiment was performed under isothermal conditions. Three different
temperatures where used. Results were collected and calculations were performed
to obtain the reaction rate constant at different temperatures and the reaction rate
constant as a function of temperature.
The first temperature was set to 250C.

 When T = 250C, y = 0.1021x - 2.0487

R² = 0.9884
k = 0.1021 s-1
The second temperature was set to 300C
 When T = 300C, y = 0.2401x - 10.305
R² = 0.99227
k = 0.2401 s-1

The third temperature was set to 350C

 When T = 350C, y = 0.4738x - 36.8

R² = 0.96436
k = 0.4738 s-1

Reaction rate constant as a function of the temperature

From y = -13723x + 43.808

Straight line equation y= mX + c

Ln K(T)= 43.808 -13723 (1/T) T=(kelvin)

Although experimental errors occurred, it’s clear that if temperature is increased, the
reaction rate constant also increases. It can be concluded that the reaction rate
constant is temperature dependent.

12
Reference
“Chemical Reactors”. 2013. The Essential Chemical Industry-Online.
http://www.essentialchemicalindustry.org/processes/chemical-reactors.html

Fogler, H. Scott. 2006. Elements of chemical reaction engineering / H. Scott Fogler.

4th ed.
ed. Upper Saddle River, NJ: Upper Saddle River, NJ : Prentice Hall PTR.

Limited, Armfield. 2013. "Transparent Batch Reactor Instruction Manual".

https://lms.curtin.edu.au/bbcswebdav/pid-5498462-dt-content-rid-
29117599_1/courses/2018_1_CHEN3010_V1_L1_A1_INT_636972/Experiment
%204%20-%20CEB-MKIII%20Issue%203%20Instruction%20Manual.pdf.

Transparent Batch Reactor Instruction Manual. 2013.

https://lms.curtin.edu.au/bbcswebdav/pid-4532836-dt-content-rid-
25220414_1/courses/302263-Cx-061-01-Sxx-x2/Experiment%204%20-
%20CEB- MKIII%20Issue%203%20Instruction%20Manual%281%29.pdf

13
Appendix
Appendix A: Data Logger Results
T= 298K

14
T= 303K

15
16
T= 308K

17
Appendix B (Nomenclature)
aµ sodium hydroxide conc. in feed bottle mol/dm3
a0 initial sodium hydroxide conc mol/dm3
a1 sodium hydroxide conc. in reactor at time t mol/dm3
a∞ sodium hydroxide conc. in reactor after ∞ time mol/dm3
b ethyl acetate conc. (same subscripts as above for mol/dm3
a)
c sodium acetate conc. (same subscripts as above mol/dm3
for a)
k specific rate constant
r reaction rate s
t elapsed time s
T reactor temperature K
V volume of reactor dm3
Xa conversion of sodium hydroxide
Xc conversion to sodium acetate
˄ conductivity S/cm
˄0 initial conductivity mS
˄1 conductivity at time t mS
˄∞ conductivity after ∞ time mS
˄a sodium hydroxide conductivity mS
˄c sodium acetate conductivity mS

18