BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 1

SAPONIFICATION REACTION OF SODIUM HYDROXIDE AND ETHYL

ACETATE IN A BATCH REACTOR

DETERMINATION OF KINETIC PARAMETERS USING BATCH REACTOR

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID
1 RADHWA BINTI MUHAMMAD FARID KA17204
2 VINODHINI A/P JAYASEELAN KA17094
3 NUR FARISAH BINTI AKMAL KA17161
4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273
5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS & DISCUSSIONS 5

4.0 CONCLUSION AND RECOMMENDATION 13

5.0 REFERENCES 14

6.0 APPENDICES 15

2
1.0 ABSTRACT

Saponification reaction is the hydrolysis of a carboxylic acid ester in a basic medium.

The role of alkali in the saponification reaction is that it breaks the ester bond and releases
the fatty acid salt and glycerol. Esters are usually present in the form of tri-glycerides.
Industrial importance of the reaction product sodium acetate demands for process
improvements in terms of maximum conversion and economical and environmental
friendly usage of raw materials. A batch reactor can be used to find the reaction rate
constant, activation energy and order of the reaction. The reaction selected in this
experiment is the liquid phase saponification reaction between sodium hydroxide (NaOH)
and (Et(Ac)) (ethyl acetate). This reaction is elementary and second-order. The objective
of the experiment is to study the effects of temperature on saponification reaction of ethyl
acetate and sodium hydroxide in batch reactor. Hence, we determine the kinetic parameters
and activation energy from this experiment. This experiment is performed in a batch reactor
and change in concentration (in terms of electrical conductivity) is measured with time at
different temperatures of 30ºC and 45ºC. At each temperature, different values of rate
constant are obtained at various time and concentration data. In this experiment, the
conductivity is recorded manually at time intervals every 2 minutes for the first 20 minutes
and every 5 minutes for the subsequent reaction time by reading the value directly from the
conductivity meter. The experiment stop when the reaction reaches steady state. It takes
shorter time for the conductivity to become constant at 45ºC compared to 30ºC which takes
around 40 minutes to become constant. To analyze our experimental data, graphical method
is used and a graph is plotted between ln (k) and 1/T and finally results shows that the value
of rate constant is find out from the graph intercept while the activation energy is calculated
from the slope of graph. The calibration curve data is also obtained by measuring the
conductivity by using the conversion between Sodium Hydroxide and Sodium Acetate.
From the result obtained, the conductivity is higher during the zero conversion where
100mL of NaOH is used.

3
 2.0 METHODOLOGY

A. Calibration Curve

250 mL NaOH, 250 mL NaOAc and 500 mL deionized water were prepared.

The solutions below were Then, each solution was mixed with 100 mL deionized water.
prepared:
-100 mL NaOH
-75 mL NaOH + 25 mL NaOAc The conductivity of each solution was recorded.
-50 mL NaOH + 50 mL NaOAc
-25 mL NaOH + 75 mL NaOAc
The reading of conductivity meter was recorded three times at
-100 mL NaOAc
different locations to find the average of conductivity values.

B. Experiment Procedure

2L of 0.1M of EtOAc and 2L of 0.1M of NaOH were prepared.

1L of each reactant solution is measured and transferred into the batch reactor via the opening at the top of
the reactor.

The temperature of reactor was set to 30oC and a thermometer was used to make sure the temperature of the
solution reached 30oC.

The stirrer was switched on at minimum speed.

The conductivity was recorded every 2 minutes for the first 20 minutes and every 5 minutes for the
subsequent reaction time until three constant readings are obtained.

Next, the liquid in the reactor was drained off.

Steps 2 to 6 were repeated using temperature at 45oC.

4
3.0 RESULTS AND DISCUSSION

3.1 Preparation of Solution for Calibration Curve

For 1 L of 0.1 M of sodium acetate For 1 L of 0.1 M of sodium hydroxide

(Na(Ac)) (NaOH)
MW of Na(Ac) = 82.03 g/mol MW of NaOH = 40.0 g/mol
Purity = 1 (as it is in solid form) Purity = 1 (as it is in solid form)
n = MV = (0.1 M)(1 L) = 0.1 mol n = MV = (0.1 M)(2 L) = 0.1 mol
m = n(MW) = 0.1 mol (82.03 g/mol) m = n(MW) = 0.1 mol (40.0 g/mol)
m = 8.203 g Na(Ac) m = 4.0 g NaOH

3.2 Preparation of Solution for Experimental Studies

For 2 L of 0.1 M of ethyl acetate (Et(Ac)) For 2 L of 0.1 M of sodium hydroxide

(NaOH)
MW of Et(Ac) = 88.11 g/mol
MW of NaOH = 40.0 g/mol
SG = 0.895 Purity = 99.5%
Purity = 1 (as it is in solid form)
Molarity of Et(Ac)
𝑆𝐺 𝑥 𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 1000 𝑔/𝐿
n = MV = (0.1 M)(2 L) = 0.2 mol
= 𝑀𝑊
m = n(MW) = 0.2 mol (40.0 g/mol)
0.895 𝑥 0.995 𝑥 1000
= m = 8.0 g NaOH
88.11

= 10.107 M
M1V1 = M2V2
10.107(V1) = 0.1 (2)
V1 = 0.0198 L= 19.80 mL of Et(Ac)

5
3.3 Calibration Curve

Table 3.1: Data for calibration curve of conversion versus conductivity

Conversion Volume of NaOH Volume of Na(Ac) Conductivity
(%) (mL) (mL) (µS/cm)
0 100 0 66.1
25 75 25 54.8
50 50 50 37.3
75 25 75 19.1
100 0 100 1.23

Table 3.2: Conductivity of product solution at 30 oC and 45 oC

Time (min) Conductivity (ms/cm) Conductivity (ms/cm)
At 30 oC At 45 oC
0 5.9 5.9
2 5.1 4.8
4 4.6 4.4
6 4.3 4.1
8 4.1 3.9
10 4.0 3.7
12 3.8 3.7
14 3.7 3.7
16 3.7 -
18 3.6 -
20 3.5 -
25 3.4 -
30 3.4 -
35 3.2 -
40 3.2 -

6
 Conversion (%)
120

100
y = -1.5011x + 103.6
R² = 0.9934
80

60

40

20

0
0 10 20 30 40 50 60 70

Figure 3.1: Calibration Curve of Conversion versus Conductivity

From Figure 3.1 above, we can see that when conductivity increases, the conversion decreases.
The ability of the electrolyte solution to conduct electricity as the solution containing anions
and cations are represented by the measured conductivity. The conductivity is also determined
by the number of charge carriers, how fast they move, and how much charge each one carries.
(Ionode Good Chemistry, 2015).The NaOH solution will form more ions to contribute more
conductivity compared to NaOAc. At zero conversion (X=0), only NaOH solution is present,
the conductivity is the highest. To sum up, the conductivity decreases when high conversion
takes place due to reduced amount of Na+ and OH- ions

7
 Conductivity (ms)
At 30 oC
7 y = -0.0519x + 4.7971
R² = 0.6996
6

0
0 5 10 15 20 25 30 35 40 45

Figure 3.2: Graph of Conductivity versus Time for Temperature of 30˚C

From Figure 3.2 above, the conductivity decreases as time increases and it achieves
steady states after an interval about 14 minutes at T=30°C. Time required for completed
reaction can be known when the values of conductivity are almost constant. This is because as
the reaction proceeds, concentration of NaOH decreases, resulting a decrease in conductivity
values.

Conductivity (ms)
At 45 oC
7
6 y = -0.1381x + 5.2417
R² = 0.7824
5
4
3
2
1
0
0 2 4 6 8 10 12 14 16

Figure 3.3: Graph of Conductivity versus Time for Temperature of 45˚C

At T=45 ˚C, the conductivity decreases as time passes. However, it achieves steady
states about after 8 seconds minutes. At higher temperature, the ions will vibrate and collide

8
faster with each other. NaOH can ionise easily to Na+ and OH- ions, and then the Na+ ions
interact with the CH3COO-ions to form sodium acetate in a faster rate since greater effective
collision make the particle easier to achieve the activation energy. The conductivity of the
solution at 30oC is higher than the conductivity at 45oC for a particular time chosen. More
NaOH are converted to product at higher temperature, hence, there are less Na+ and OH- ions
left in the solution to conduct electricity. The higher temperature results in higher conversion
of reactants and lower conductivity values

Question 1

I) Describe how do you find order of a reactant using differential/integral method of

analysis? Give the graph that would be used to prove that the reaction is first order with
respect to both NaOH & EtOAc.

Chemical equation: NaOH + EtOAc→ NaOAc + EtOH

A+B→C+D
If the reaction is first order with respect to both NaOH & EtOAc, which mean that the overall
order of the reaction is 2nd order. According to Fogler (2014), by using integral method, we
should obtain a linear graph when 1/CA versus t is plotted using experimental data, provides
that it is a second order reaction.
Derivations of equations are shown as below second order reaction:

Since the stoichiometric coefficient for A and B are the same, hence CA =CB.

y = mx + c

9
 Figure 3.4: Graph of 1/CA versus Time

Firstly, use the equation in Figure 3.1 to find the value of unknown conversion in the data set
of Table 3.2. After obtaining the conversion values for each data for both temperatures, hence
get the concentration amount with respect of conversion. In term of 1/Ca, a graph of 1/Ca vs
time can be plotted to show the trend of a second order equation.

Cao = 1000 mol/m3, by dividing number of mol with volume.

Ca = Cao (1-x)

Table 3.3: Conversion vs Volume

x
(%) V(mL) V(L) V(m3)
0 100 0.1 0.0001
25 75 0.075 0.000075
50 50 0.05 0.00005
75 25 0.025 0.000025
100 0 0 0

10
 Table 3.4: Conversion, Concentration and 1/Ca value with time at 30C
Conversion, Conversion, x Ca 1/Ca Time
x (%) Conductivity, mS
0.947435 94.74351 5.9 52.5649 0.019024 0
0.959444 95.94439 5.1 40.5561 0.024657 2
0.966949 96.69494 4.6 33.0506 0.030257 4
0.971453 97.14527 4.3 28.5437 0.030257 6
0.974455 97.44549 4.1 25.5451 0.03503 8
0.975956 97.5956 4 24.044 0.039146 10
0.978958 97.89582 3.8 21.0418 0.04159 12
0.980459 98.04593 3.7 19.5407 0.047524 14
0.980459 98.04593 3.7 19.5407 0.051175 16
0.98196 98.19604 3.6 18.0396 0.051175 18
0.983462 98.34615 3.5 16.5385 0.055434 20
0.984963 98.49626 3.4 15.0374 0.060465 25
0.984963 98.49626 3.4 15.0374 0.066501 30
0.987965 98.79648 3.2 12.0352 0.066501 35
0.987965 98.79648 3.2 12.0352 0.08309 40

1/Ca vs time at 30◦C

0.1
0.09 y = 0.0016x + 0.025
0.08
0.07
0.06
1/Ca

0.05
0.04
0.03
0.02
0.01
0
0 5 10 15 20 25 30 35 40 45
Time (min)

Figure 3.5: 1/Ca vs Time (min) at 30C

11
 Table 3.5: Table of Conversion, Concentration, 1/Ca with time at 45C
Conductivity Time
x (%) x Ca 1/Ca (mS)
94.74351 0.947435 52.5649 0.019024 5.9 0
96.39472 0.963947 36.0528 0.027737 4.8 2
96.99516 0.969952 30.0484 0.03328 4.4 4
97.44549 0.974455 25.5451 0.039146 4.1 6
97.74571 0.977457 22.5429 0.04436 3.9 8
98.04593 0.980459 19.5407 0.051175 3.7 10
98.04593 0.980459 19.5407 0.051175 3.7 12
98.04593 0.980459 19.5407 0.051175 3.7 14

1/Ca vs Time at 45 C
16
14
12
y = 389.9x - 8.4533
10
8
1/Ca

6
4
2
0
0 0.01 0.02 0.03 0.04 0.05 0.06
-2
Time (min)

Figure 3.6: 1/Ca vs Time at 45C

Both graphs show the trend of a second order equation derivations at both 30 and 45 degree
Celsius respectively.

12
4.0 CONCLUSION

As a conclusion, in this experiment, we can conclude that the temperature plays an

important role in the saponification reaction of ethyl acetate and sodium hydroxide in a batch
reactor. The higher the temperature, the higher the conductivity. This can be proven by looking
Table 2.1 and Table 2.2. The value of conductivity at 30°C is higher than the conductivity at
45°C. This also shows that temperature increases the rate of reaction. From the experiment, the
value of 1/CA increased directly with time, which indicates this is a first order for both
temperatures.

The result showed a very large derivation from literature value as there are few factors
that may have caused the error. It was suggested that the main reason for the difference was
the method of plotting calibration curve. The method of determining conversion using
conversion did not take into account the effect of temperature and imperfect mixing caused a
major difference in the result.

For recommendations, to ensure accuracy and safety of the experiment, the conductivity
meter should be well calibrated before being used to reduce instrumentation error. Besides, the
conductivity meter must also be rinsed with the water after taking each reading. Moreover, the
batch reactor must first be purged with the pure water (wash) to remove and flash out the
contaminants which might cause deviation in conductivity reading. To speed up the heating or
cooling process, the solution of thermostat bath can be changed to other solution as well.
Besides, for experiment at 45°C it was suggested to take the reading at a shorter interval as the
reaction ended very fast, hence taking a shorter interval reading may result in a more accurate
result especially when plotting graph to determine the rate constant. The reading at time, t = 0
should be taken by either preparing another entrance to insert conductivity meter or install a
conductivity transmitter in the reactor to ease the reading taking.

13
5.0 REFERENCES

1. Fogler, H. Scott (2014), Elements of Chemical Reaction Engineering 4th Ed., New York,
Pearson Education Ltd.

2. Kuheli Das, P., Sahoo, M., Sai Baba, N., Murali, P., & Swaminathan (2011), Kinetic Studies
on Saponification of Ethyl Acetate Using an Innovative Conductivity-Monitoring Instrument
with a Pulsating Sensor, Wiley Online, 1-8.

14
6.0 APPENDICES

Figure 6.1: Results for calibration curve

Figure 6.2: Results for conductivity of solution

15
 BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 2

CONTINUOUS STIRRED REACTION

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID
1 RADHWA BINTI MUHAMMAD FARID KA17204
2 VINODHINI A/P JAYASEELAN KA17094
3 NUR FARISAH BINTI AKMAL KA17161
4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273
5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS AND DISCUSSIONS 6

4.0 CONCLUSION AND RECOMMENDATION 14

5.0 REFERENCES 15

6.0 APPENDICES 16

2
1.0 ABSTRACT

The study is carried out for the sodium hydroxide and ethyl acetate saponification reaction
in a CSTR reactor. The goal of the experiment was to research the effects of the reactant flow
rate on CSTR and the effectiveness yield of CSTR saponification, Et(Ac) and Sodium
hydroxide. Before we start the experiment, calibration curve for a graph of conversion versus
conductivity by using sodium hydroxide, NaOH and sodium acetate, NaOAc need to be
prepared.
Calibration curve of conversion versus conductivity was prepared by using 100ml, 75ml,
50ml, 25ml and 0ml of sodium hydroxide to get 0% conversion to 100% conversion
conductivity reading. In the experiment, 10L of 0.1M Et(Ac) and 10L of 0.1M NaOH was
prepared for feed tanks T1 and T2. The first experiment flow rate of both tanks was set to 100
mL/min initially and stirrer were set to 200 rpm. The conductivity values (CT1, CT2 & CT3)
and temperature values (TT1, TT2 & TT3) were recorded every 2 minutes until steady state.
Then, the experiment was repeated with a different flow rate of 150 mL/min. From the
calibration curve gained, conductivity value is inversely proportional with conversion. The
conductivity value decreases as the conversion increases.
From the result, it was found out that conversion, X at flowrates 100mL/min in CT3 showed
a higher value than that at 150mL/min in CT3 in steady state. The result shows that the higher
the flow rate of reactor, the higher the conductivity of the solution. This is because when the
volumetric flow rate increases, the residence time of the reagents in the reactors will decreases.
Therefore, the rate of reaction will be decreased. Hence, the yield of the saponification of the
CSTR decreases as the volumetric flow rate increases.

3
2.0 METHODOLOGY

2.1 PREPARATION OF CALIBRATION CURVE FOR CONVERSION VS.

CONDUCTIVITY

The conductivity for

each conversion values
by mixing the
following solutions
into 100 mL of
deionised water is
determined.
10-L of 0.1M sodium i- 100 mL NaOH for
The calibration curve
hydroxide (NaOH) 0% conversion
of conversion vs.
solution and 10-L of ii- 75 mL NaOH + 25
conductivity is plotted.
0.1M sodium acetate mL Na(Ac) for 25%
The slope and y-axis
(Na(Ac)) solution is conversion
intersept is determined.
prepared. iii- 50 mL NaOH + 50
mL Na(Ac) for 50%
conversion
iv- 25 mL NaOH + 75
mL Na(Ac) for 75 %
conversion
v- 100 mL Na(Ac) for
100% conversion

4
2.2 SAPONIFICATION OF CSTR IN SERIES

The 3-way valve V1 was position

10-L of 0.1M Et(Ac) solution is 10-L of 0.1 M NaOH solution is
towards pump P1 and 3-way valve
charged into feed tank T1. charged into feed tank T2.
V2 was position towards pump P2.

The needle valves V3 and V4 is

adjusted to obtain flowrates of
approximately 100 mL/min on both
Valves V3, V4 and V5 is opened. Pumps P1 and P2 is switched on. flowmeters FT1 and FT2. The
flowrates are always maintained the
same and there were no air bubbles
were trapped in the piping.

The conductivity values (CT1, CT2

and CT3) and temperature values
Both liquids were allowed to fill up (TT1, TT2 and TT3) is monitored
all three reactors. Stirrers 1, 2 and 3 every two minutes until they do not
was switched on and the stirrer The timing was started and taken. change over time (steady state). The
speeds was set to approximately 200 timing is stooped recorded with it
rpm. conductivity values. The conversion
in each reactors from the calibration
curve is determined.

The experiment (steps 6 to 9) is

repeated by changing the flowrate to
150mL/min.

5
3.0 DISCUSSIONS

3.1 RESULT

(A) Preparation of Solution for Calibration Curve

For 1 L of 0.1 M of sodium acetate (Na(Ac)) For 1 L of 0.1 M of sodium hydroxide (NaOH)
MW of Na(Ac) = 82.03 g/mol MW of NaOH = 40.0 g/mol
Purity = 1 (as it is in solid form) SG= 1.483 Purity = 45%
n = MV = (0.1 M)(1 L) = 0.1 mol Density of water (4oC) = 1kg/L = 1000 g/L
m = n(MW) = 0.1 mol (82.03 g/mol) 𝑆𝐺 𝑥 𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 1000 𝑔/𝐿
Molarity of NaOH =
𝑀𝑊
m = 8.203 g Na(Ac)
1.483 𝑥 0.45 𝑥 1000
=
40
= 16.7 M
M1V1 = M2V2
16.7(V1) = 0.1 (1)
V1 =0.00599 L = 5.99 mL of NaOH

(B) Preparation of Solution for Experimental Studies

For 10 L of 0.1 M of ethyl acetate (Et(Ac)) For 10 L of 0.1 M of sodium hydroxide (NaOH)
MW of Et(Ac) = 88.11 g/mol MW of NaOH = 40.0 g/mol
SG = 0.895 Purity = 99.5% SG= 1.483 Purity = 45%
Molarity of Et(Ac) Molarity of NaOH
𝑆𝐺 𝑥 𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 1000 𝑔/𝐿 𝑆𝐺 𝑥 𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 1000 𝑔/𝐿
= = 𝑀𝑊
𝑀𝑊
1.483 𝑥 0.45 𝑥 1000
0.895 𝑥 0.995 𝑥 1000 = 40
=
88.11
= 16.7 M
= 10.107 M
M1V1 = M2V2
M1V1 = M2V2
16.7(V1) = 0.1 (10)
10.107(V1) = 0.1 (10)
V1 =0.0599 L= 59.88 mL of NaOH
V1 = 0.0989 L= 98.9 mL of Et(Ac)

6
Temperature of CSTR = 29oC (constant throughout the experiment)

Table 1: Data for calibration curve of conversion versus conductivity

Conversion Volume of NaOH Volume of Na(Ac) Conductivity

(mL) (mL) (mS/cm)
0 100 0 1.23
25 75 25 9.10
50 50 50 37.3
75 25 75 54.8
100 0 100 66.1

Flow rate = 100mL/min

Temperature (OC) Conductivity (mS/cm)
Time TT1 TT2 TT3 CT1 CT2 CT3
(min)

0 23.3 23.8 23.9 0.01 0.06 0.02

2 23.4 24 23.1 7.75 2.4 0.02
4 23.4 24.1 24.1 9.15 3.2 0.02
6 23.4 24.1 24.1 10.4 5.8 0.02
8 23.4 24.1 24 11 6.7 0.02
10 23.5 24.3 24.1 11.28 8.7 0.02
12 23.5 24.3 24.1 11.48 9.8 4.3
14 23.5 24.3 24.2 11.68 10.2 4.5
16 23.6 24.4 24.2 11.7 10.35 5
18 23.6 24.4 23.6 11.88 10.88 6.32
20 23.6 24.5 24.3 11.69 11.28 8.45
22 23.7 24.5 24.4 12.04 11.66 9.09
24 23.7 24.5 24.4 12.11 11.94 9.4
26 23.7 24.5 24.4 12.16 12.17 9.74
28 23.7 24.5 24.4 12.2 12.36 10
30 23.7 24.5 24.4 12.25 12.46 10.24

7
Flow rate = 150mL/min
Temperature (OC) Conductivity (mS/cm)
Time TT1 TT2 TT3 CT1 CT2 CT3
(min)

0 23.8 24.6 24.5 12.25 12.2 10.45

2 23.8 24.7 24.5 12.35 12.21 10.75
4 23.9 24.7 24.5 12.41 12.3 11
6 23.9 24.7 24.6 12.42 12.32 11.11
8 24 24.8 24.6 12.5 12.4 11.12
10 24 24.8 24.7 12.52 12.42 11.2
12 24 24.8 24.7 12.54 12.43 11.21
14 24 24.9 24.7 12.56 12.45 11.22
16 24.1 25 24.8 12.56 12.46 11.23
18 24.2 25 24.8 12.58 12.5 11.24
20 24.2 25 24.9 12.60 12.6 11.24
22 24.2 25.1 24.9 12.63 12.61 11.24
24 24.3 25.2 24.9 12.67 12.63 11.11
26 24.3 25.3 25 12.67 12.65 11.11
28 24.3 25.3 25 12.8 12.7 11.10
30 24.4 25.4 25 13 12.75 11.11

3.2 DISCUSSION

1. Plot the calibration curve of conversion vs. conductivity and discuss relationship
between these parameters.

Good conductor of electricity contains charged particles that are free to move. For salt
solution of sodium acetate, the ions represent charged particles with relatively high mobility,
in another words high ability to move. Theoretically, conductivity should increase as
concentration of the dissolved salt in water increases due to increase in conversion of NaOH.
The concentration and mobility of the ions are not independent properties. As the
concentration of an ion increases, its mobility decreases (Jack,2018). The line equation
obtained for the relationship between conversion and conductivity is y = 1.3847x + 3.3261.

8
 Graph of Conversion vs Conductivity
120

100 y = 1.3847x + 3.3261 100

80
75

60
50
40

25
20

0 0
0 10 20 30 40 50 60 70

Figure 3.1: Graph of Conversion vs Conductivity

2. Plot a graph of conductivity/conversion vs. time for each flow rate. Discuss a plotted
graph and make a comparison n term of conversion for each flow rate.

Conduction vs Time
14

12

10
Conduction

0
0 5 10 15 20 25 30 35
Time

CT1 CT2 CT3

Figure 3.2: Graph of Conduction vs Time at 100 mL/min

9
 15
Conduction

10

0
0 5 10 15 20 25 30 35
Time

CT1 CT2 CT3

Figure 3.3: Graph of Conduction vs time at 150 mL/min

From Figure 3.2 and Figure 3.3, the conductivity is higher at the volumetric flow rate of
150ml/min than the volumetric flow rate of 100ml/min. But for the space time for 100ml/min
is higher than 150ml/min. Residence time is the average amount of time that a discrete quantity
of reagents spent inside the tank. (Fogler, 2004) When the volumetric flow rate increases, the
space time of the reagents in the reactors will be reduced. Hence, the rate of reaction will be
decreased. This is because fewer reagents are converted into products.

10
3. Plot a graph of conductivity/conversion vs. time for single reactor of each flowrate.
Discuss a plotted graph and make a comparison in term of conversion for each flowrate.

Graph of conversion vs time for C1

70
60
Conversion (%)

50
40
30
20
10
0
0 2 4 6 8 10 12 14 16 18 20
Time (min)

100 mL/min 150 mL/min

Figure 3.4: Graph of conversion versus time for C 1

Graph of conversion vs time for C2

80
70
60
Conversion (%)

50
40
30
20
10
0
0 2 4 6 8 10 12 14 16 18 20
Time (min)

100 mL/min 150 mL/min

Figure 3.5: Graph of conversion versus time for C 2

11
 Graph of conversion vs time for C3
85

80
Conversion (%)
75

70

65

60
0 2 4 6 8 10 12 14 16 18 20
Time (min)

100 mL/min 150 mL/min

Figure 3.6: Graph of conversion versus time for C 3

Graph of conversion vs time for C4

90
80
70
Conversion (%)

60
50
40
30
20
10
0
0 2 4 6 8 10 12 14 16 18 20
Time (min)

100 mL/min 150 mL/min

Figure 3.7: Graph of conversion versus time for C 4

From Figure 3.1 to Figure 3.4, we can clearly observe that the conversion of sodium hydroxide
is higher with a flow rate of 100 mL/min than flow rate of 150 mL/min. The higher the flow
rate, the lower the conversion of sodium hydroxide. In steady state, there should be no changes
in the conductivity and conversion in the Continuous Stirred Tank Reactor (CSTR) with time.
However, there are some fluctuation occur due to some errors during the experiment. Besides,
lab assistant mentioned that the conductivity measured by controller 3 and controller 4 should
be the same because they are from the same outlet stream. Hence, we suspect that the result of
controller 3 and controller 4 have some deviation.

12
4. Give the advantages of CSTR and compare with other types reactors.

The advantages of CSTR are it is relatively cheaper and simpler to be constructed

compare to other reactors such as batch reactor and PFR. It is also easier in controlling
temperature in each stage since each stage operate in a stationary state. The heat transfer surface
for this reactor can be easily provided and can be readily adapted for automatic control in
general that allowing fast response to changes in operating conditions for examples, feed rate
and its concentration. (Zulkipeli, 2015).

5. Give several applications of CSTR in chemical processor industries (at least 3

applications)

Continuously stirred tank bioreactor (CSTR) is used to optimize feasible and reliable
bioprocess system in order to treat hydrocarbon-rich industrial wastewaters. Besides, CSTRs
are used in industrial processing, primarily in homogeneous liquid-phase flow reactions, where
constant agitation is required. They may be used by themselves, in series, or in a battery. CSTR
are also used in the pharmaceutical as a loop reactor. CSTRs are often used in biological
processes, such as cell cultures. (Ren, N.-Q et al, 2010)

13
4.0 CONCLUSION AND RECOMMENDATIONS

After the experiment has been conducted, the outcome results give the strong evidence
that both the objectives of this experiment were successfully achieved. First objective is to
study the effect of reactant flow rate on saponification of ethyl acetate and sodium hydroxide
in CSTR. Based on the figure conversion versus time at flow rate 100 mL/min and 150 mL/min
for each controller above indicates that the lower the flow rate, the higher the conversion of
sodium hydroxide can be achieved. In the first place, Fogler (2014) provided that for a multiple
continuous stirred tank reactor that connected in a series manner, each subsequent reactors will
achieve a higher conversion than the preceding reactors as it continue to convert unreacted
reactant into product. Results obtained for 100 mL/min flow rate specifically give the final
values of 12.25, 12.46 and 10.24 mS/cm for controller 1, controller 2 and collector 3
respectively. In the other hand, 150 mL/min flow rate gives the final conductivity values of 13,
12.75 and 11 mS/cm.

To avoid error in the readings, the concentration of ethyl acetate stock solution and
volume required for its dilution must be calculated correctly. If the calculation was wrong, the
concentration of the diluted ethyl acetate will be different from the required concentration.
Besides, the conductivity meter also must be handled with care since the readings can be
slightly deviate due to mishandle of the equipment. Before the conductivity value of each
sample is taken, the probe is rinsed with distilled water to avoid contamination to the reaction
of sodium hydroxide and ethyl acetate being converted into sodium acetate.

14
5.0 REFERENCES

• Lehigh University. (2015). About Conductivity. Retrieved from

http://www.lehigh.edu/~amb4/wbi/kwardlow/conductivity.htm
• Fogler, H.S. (2014). Elements of Chemical Reaction Engineering. (4thed). USA:
Pearson Education Limited.

• Hojo, O., Hokka, C., & Major, A. (1999). Ethanol production by a flocculant yeast
strain in a CSTR type fermentor with cell recycling. pp. 535-45.

• Mohd Danish et al. (2015, February). Effect of Operating Conditions on CSTR

performance: an. Int. Journal of Engineering Research and Applications, 5(2), 74-78.

• Ren, N.-Q., Tang, J., Liu, B.-F., & Guo, W.-Q. (2010, April). Biological hydrogen
production in continuous stirred tank reactor systems with suspended and attached
microbial growth. International Journal of Hydrogen Energy, 35(7), 2807–2813.

• Zulkipeli, A. (2011, February 26). Advantages and Disadvanteges of a CSTR.

Retrieved from https://www.scribd.com/doc/49597945/ADVANTAGES-AND-
DISADVANTAGES-OF-A-CSTR

15
6.0 APPENDICES

16
17
 BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 3

THE EFFECT OF MEAN RESIDENCE TIME ON PLUG FLOW REACTION

PROCESS

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID
1 RADHWA BINTI MUHAMMAD FARID KA17204
2 VINODHINI A/P JAYASEELAN KA17094
3 NUR FARISAH BINTI AKMAL KA17161
4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273
5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS AND DISCUSSIONS 5

4.0 CONCLUSION AND RECOMMENDATION 11

5.0 REFERENCES 12

2
1.0 ABSTRACT

In the chemical industry, the Plug Flow Reactor is commonly used. The benefits of the
PFR reactor are that the plug flow reactors have a high conversion volumetric unit and operate
without maintenance for long periods of time. A issue often found in the chemical industry is
the control of the Plug Flow Reactor system. Due to the time-varying and nonlinear features of
the plug flow reactor systems, the regulation of the plug flow reactor in chemical industries is
very difficult. The plug flow reactor (PFR) phase model nonlinear model is used to When using
a continuous tubular reactor to achieve a specified output, estimate the main unit activity
variables. This paper offers a description of the selection of the best model for designing a
nonlinear plug flow reactor model. The steps in designing a nonlinear plug flow reactor model
are to build a first principal mathematical model, including simulation under the plug flow
reactor. Steady state and chaotic state condition, an experimental validation of the
mathematical model.

A plug flow reactor was used in this experiment to research the influence of average
residence time on the conversion factor of the ethyl acetate and sodium hydroxide
saponification reaction. With a molarity of 0.1 molar for ethyl acetate and sodium hydroxide
formula, a solution for saponification reaction was prepared. Three separate flow rates of 2 L/h,
4 L/h and 6 L/h will manipulate the flow rate for all of these solutions. The reading of the
effluent is taken every 2 minutes to calculate the conductivity until it is steady. Several
difficulties arose during the execution of the experiment and have been addressed in this article.
It indicates that the conversion decreases as the conductivity decreases on the basis of the
results of the experiment. In the debate, the aspects of this experiment were clarified.

3
 2.0 METHODOLOGY

2.1 PREPARATION OF CALIBRATION CURVE FOR CONVERSION VS.

CONDUCTIVITY

The conductivity for each conversion value was

determined by preparing 100ml as following :
1L of 0.1M sodium
hydroxide (NaOH) i. 100 mL NaOH for 0% conversion
solution and 1L of 0.1M ii. 75 mL NaOH +25 mL Na(Ac) for 25 % conversion
sodium acetate (Na(Ac)) iii. 50 mL NaOH + 50 mL Na(Ac) for 50% conversion
solution were prepared.
iv. 25 mL NaOH + 75 mL Na(Ac) for 75 % conversion
v. 100 mL Na(Ac) for 100% conversion

10 L of 0.1 M ethyl acetate and 10 L of 0.1 M sodium hydroxide were prepared and poured into
corresponding reactant tanks.

The main switch was switched on. The required temperature of water that will be as same as reactor and
reactant temperature was set at 35oC.

The dosing pump 1 and dosing pump 2 were switched on and flow rate was set at 2 L/hr. Stop watch was
started.

The conductivity values for the product stream was monitored whe the products are coming out from the
reactor. The reading was recorded down every 2 minutes until the detected conductivity does not change
over time. The stop watch was paused and the time was recorded.

The experiment was repeated for different flow rates by setting the flow rate of dosage pumps to 4 L/hr
and 6 L/hr.

The residual liquid from the reactor was drain off and the reactor and tubings are properly cleaned after
completing the experiment.

All liquid was disposed immediately after each experiment. Do not leave any solution or waste in tanks
over a long period of time.

Any spillage from the experimental unit was wiped off immediately.

4
3.0 DISCUSSIONS

Table 3.1 : Preparation for calibration curve

For 1L of 0.1M sodium acetate (Na(Ac)) For 1 L of 0.1 M of sodium hydroxide (NaOH)

MW of (Na(Ac)) = 82.03 g/mol MW of NaOH = 40.0 g/mol

Purity = 1 (solid form) Purity = 1 (pellet form)
n = MV = (0.1 M) (1 L) = 0.1 mol n = MV = (0.1 M) (1 L) = 0.1 mol
m = n(MW) = (0.1 mol) (82.03 g/mol) m = n(MW) = (0.1 mol) (40.0 g/mol)
= 8.203 g Na(Ac) = 4 g NaOH

Table 3.2: Preparation for ethyl acetate and sodium hydroxide

For 10L of 0.1M ethyl acetate (Et(Ac)) For 10L of 0.1 M of sodium hydroxide
(NaOH)
MW of (Na(Ac)) = 88.1 g/mol
SG= 0.895 MW of NaOH = 40.0 g/mol
Purity = 99.5% Purity = 1 (pellet form)
Molarity of Et(Ac) n = MV = (0.1 M)(10 L) = 1.0 mol
= 𝑆𝐺 𝑋 𝑃𝑢𝑟𝑖𝑡𝑦 𝑋 1000 𝑔/𝐿𝑀𝑊 m = n(MW) = (1.0 mol)(40.0 g/mol)
= 0.895 𝑋 0.995 𝑋 1000 88.11 = 40 g NaOH
= 10.11 M
M1V1 = M2V2
10.11(V1) = 0.1 (10)
V1 = 0.0989 L = 98.9 mL of Et (Ac)

5
 Table 3.3: Table for Calibration Curve of Conversion Versus Conductivity

Conversion Volume of NaOH Volume of Na(Ac) Conductivity

(mL) (mL) (mS/cm)
0 100 0 1.23
25 75 25 9.10
50 50 50 37.3
75 25 75 54.8
100 0 100 66.1

Table 3.4: Conductivity at different flow rate

Conductivity (mS/cm)
Time (min)
2 L/h 4 L/h 6 L/h
0 3.4 1.9 2.2
2 2.6 1.8 2.5
4 2.3 2.0 2.5
6 2.1 2.1 2.5
8 2.0 2.2 -
10 1.9 2.2 -
12 1.9 2.2 -
14 1.9 - -

6
3.2 DISCUSSIONS

Graph of Conversion vs Conductivity

120

100 y = 1.3847x + 3.3261 100

80
Conversion

75
60
50
40
25
20

0 0
0 10 20 30 40 50 60 70
Conductivity

Figure 3.1: Graph of Conversion vs Conductivity

From Figure 3.1, we can conclude that conversion is directly proportional to conductivity. As
higher conversion is reached, less freely-moving Na+ and OH- ions are being converted into
NaAc, which has very high dissociation in water to produce freely-moving ions. The increase
of freely-moving, electroconductive ions explains why conductivity increase at high
conversion. The relation between conversion and conductivity can be presented by the
correlation y = 1.3847x + 3.3261, with x represent conductivity and y represent conversion.

1. Plot a graph of conductivity/ conversion vs. time for each flow rate. Discuss the
plotted graph and make comparison in terms of conversion for each flow rate.

By using the relation between conversion and conductivity can be presented by

the correlation y = 1.3847x + 3.3261. The conversion for each flow rate can be obtained
by substituting the value of conductivities.

7
 Table 3.5: Conversion versus time at different flow rate

Conversion , X
Time (min)
2 L/h 4 L/h 6 L/h
0 8.0341 5.9570 6.3724
2 6.9263 5.8186 6.7879
4 6.5109 6.0955 6.7879
6 6.2340 6.2340 6.7879
8 6.0955 6.3724 -
10 5.9570 6.3724 -
12 5.9570 6.3724 -
14 5.9570 - -

Conversion versus Time

9
8
7
Conversion, X

6
5
2 L/h
4
4 L/h
3
6 L/h
2
1
0
0 2 4 6 8 10 12 14 16
Time (min)

Figure 3.2: Graph of Conversion versus Time for Different Flow Rate

On the basis of the above figure, it is easy to see that the different
conductance/conversion results over time at various flow speeds. Conversion is directly
proportional to conductivity, as we know from the calibrating curve. The conductivity values
increase throughout the whole time as the conversions increase. Based on our experiment, the
conversion of the reactants is the highest at the flow rate of 2L/h at around 5.9-8.0%. On the
other hand, the conversions for the flow rates of 4L/h are in the range of 5.8-6.4% while for
the 6L/h the conversions are in the range of 6.4-6.8%. This is due to the effect of mean
residence time. Mean residence time is defined as the average amount of time that the reactants

8
spent in the reactor. When the flow rate is low, the reactants can spend more time in the reactor
before leaving and it will help to increase the conversion. Thus, the conversion will increase
when the flow rates decrease.

2. Suggest other parameters which can also be used to monitor the reaction and give
your justification.

To monitor the reaction, temperature may be used. The molecules in the solution gain
energy as the temperature rises and collide most frequently with other molecules. The effective
collision of the molecules also increases the reaction rate. In addition, catalyst usage can be
used to control the influence of a reaction as a parameter. The catalyst purpose of the reactor
is to provide an alternative means of minimising the activation energy required for the
compound to be overcome by the reactants. It helps to increase the substance produced in a
reaction by adding catalyst.

3. Give 3 advantages of Tubular Reactor.

Tubular reactors have a wide variety of applications in either gas or liquid phase
systems. There are several advantages in using Tubular Reactor as it have high conversion rate
per reactor volume. The reactor can be easily maintained since there are no moving parts which
make the reactor is mechanically simple. Other than that, this reactor is suitable for large
capacity processes and the product quality are unvaried. Common industrial uses of tubular
reactors are in gasoline production, oil cracking, synthesis of ammonia from its elements, and
the oxidation of sulphur dioxide to sulphur trioxide.

4. What are the differences between Tubular Reactor and Continuous Stirred Tank
Reactors?

The main difference between Tubular Reactor and Continuous Stirred Tank Reactor
(CSTR) are the tubular reactor has a higher theoretical efficiency than a CSTR of the same
volume. That the given same space-time or residence time, a reaction will proceed to a higher
percentage completion in a tubular reactor than in a CSTR.

9
 In a tubular reactor, one or more fluid reagents are pumped through a pipe or tube. The
chemical reaction proceeds as the reagents travel through the tubular reactor. In this type of
reactor, the changing reaction rate creates a gradient with respect to distance traversed; at the
inlet to the reactor the rate is very high, but as the concentrations of the reagents decrease and
the concentration of the product increases the reaction rate slows.

In a CSTR, one or more fluid reagents are introduced into a tank reactor which is
typically stirred with an impeller to ensure proper mixing of the reagents while the reactor
effluent is removed. Dividing the volume of the tank by the average volumetric flow rate
through the tank gives the space time, or the time required to process one reactor volume of
fluid. Using chemical kinetics, the reaction's expected percent completion can be calculated.
All calculations performed with CSTRs assume perfect mixing.

5. How can you know that the reaction has reached the steady state?

When a reaction involves one or more intermediates, the concentration of one of the
intermediates remains constant at some stage of the reaction. Thus, the system has reached a
steady-state. We can know from this experiment that when the conductivity shows same
reading three times, we can assume that it have reached.

10
4.0 CONCLUSION AND RECOMMENDATIONS

From the result that we have been obtained in the experiment of Plug Flow Reactor (PFR),
we can conclude that the conductivity are influences by the flow rate of reaction. Initially, the
flow rate is set at 2 L/hour. Then, the conductivity value is measure until it reaches constant
reading. For 2 L/hour flow rate it takes longer time to get the constant conductivity reading. It
is because it takes longer time to react inside the reactor. The experiment was continued with
different flow rate which is 4 L/hour and 6 L/hour. For 6 L/hour it takes the fastest time to get
the constant conductivity reading, because it takes shortest time to react inside the reactor.

We have discovered that some precautions should be taken into consideration when running
the experiment. The sensor of the conductivity meter should be dipped into distilled water after
every reading were taken to decrease the error of the results. Besides that, the pipes of the PFR
should be cleaned and the mixture of reactants and the products in the pipes should be purged
out. This is done to ensure that every reaction started from the beginning. Other than that, we
need to make sure that the solution that we prepared are not contaminated.

11
5.0 REFERENCES

H. Scott Fogler. (2006). Elements of Chemical Reaction Engineering (4th ed.). United States:
Pearson International Edition.

12
 BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 4

HETEROGENEOUSLY CATALYZED HYDROLYSIS OF ETHYL ACETATE IN

PACKED BED REACTOR

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID
1 RADHWA BINTI MUHAMMAD FARID KA17204
2 VINODHINI A/P JAYASEELAN KA17094
3 NUR FARISAH BINTI AKMAL KA17161
4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273
5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS AND DISCUSSIONS 5

4.0 CONCLUSION AND RECOMMENDATION 12

5.0 REFERENCES 13

6.0 APPENDICES 14

2
1.0 ABSTRACT

Catalytic Packed Bed Reactor (PBR) has been designed for experiments on chemical
reaction in liquid phase under isothermal and adiabatic condition. These reactors are tubular
and are filled with solid catalyst particles, most often used to catalyse gas reactions. The three
objectives of this experiment is to determine the reaction rate constant, to study the effect of
residence time on the conversion and lastly to determine the bed voltage using experimental
rig. The first experiment were to prepared a calibration curve for conversion vs. conductivity.
Firstly 1 L of 0.1 M CH3COOH and 0.1 M EtAc were prepared. Then both solution were mixed
together in a different amount at different conversion which is 25%, 50%, 75% and 100%. The
conductivity for each conversion were determined by using conductivity meter. The second
experiment were to determine the rate constant in batch mode. Firstly 250 mL ethyl acetate
were measured in 500 mL beaker. Then 1g of pre-swelled catalyst were added to the beaker
under vigorous stirring using th magnetic stirrer. The initial conductivity were recorded. Then
every two minutes of time interval the conductivity were recorded using conductivity meter.
The rate constant then determined using differential or integral method. The final experiment
were PBR operation and this experiment need to be done three times using flow rate of 20, 30
and 40 mL/min. Firstly the general start-up procedure were performed and then open valve V1
and V4. Then allowed EtAc to enter the reactor and after that the flowrate controller were
adjusted to give a constant flow rate of 20 mL/min. The reactor inlet and outlet were connected
to the manometer once the reactant solution passes through the reactor in order to measure the
pressure drop. The conductivity of the product were measured and recorded for every 1 minutes
until the conductivity readings remain constant. The experiment were then repeated using the
other flow rate.

3
2.0 METHODOLOGY
Part A: Preparation of Calibration Curve for Conversion VS Conductivity

3 L of 0.4 M ethyl acetate (EtAc) solution and 1 L of 0.4 M acetic acid

(HAc) solution were prepared.

The conductivity for each conversion value was

determined by prepared 100 ml of the following solution.
• 1) 100 ml of EtAc [X = 0%]
• 2) 75 ml of EtAc & 25 ml of HAc [X = 25%]
• 3) 50 ml of EtAc & 50 ml HAc [X = 50%]
• 4) 25 ml of EtAc & 75 ml of HAc [X = 75%]
• 5) 100 ml of HAc [X = 100%]
• where X is the conversion

Part B: Experiment Procedure for PBR operation

The flowrate controller was
3L of 0.4M ethyl acetate Valve V1 and V2 was adjusted to give a constant
solution was prepared opened. Ethyl Acetate flowrate of 20 mL/min. The
reactor inlet and outlet was
and the Tank B1 was solution was allowed to connected to the manometer to
filled. enter the tubular reactor. measure the pressure drop once the
reactant passes through the reactor.

The conductivity of the feed The steady state conductivity Step 2 to 4 was repeated for
solution was recorded and values at the inlet and outlet was
different residence time by
the conductivity effluent at recorded. The concentration of
acetic acid exiting the reactor changing the feed flow rates
outlet was monitored at
several times until it became and extent of conversion from of ethyl acetate to 30 ml/min
steady. calibration curve was calculated. and 40 ml/min.

Part C: Experimental Procedure For the Determination of Rate Constant in Batch

Mode

The conductivity if the initial

1g of the pre-swelled catalsyt
250mL of 0.4M Ethyl was recorded at different
(dry weight) was added to the
Acetate solution was time interval samples. The
beaker under vigorous
measured in 500mL in specific rate constant was
stirring using the magnetic
beaker. determined using differential
stirrer.
or integral method.

4
3.0 RESULTS AND DISCUSSIONS

3.1 RESULTS

PBR OPERATOR DATA RESULT

Table 3.1 Conductivity versus time at different flow rate

Flow Rate
20 30 40
(mL/min)
Conductivity of the efficient at
Time (min)
outlet (mS/cm)
0 - - -
2 0.91 0.47 0.43
4 0.84 0.46 0.39
6 0.78 0.45 0.38
8 0.7 0.44 0.37
10 0.66 0.43 0.37
12 0.55 0.42 0.37
14 0.47 0.41 -
16 0.41 0.41 -
18 0.41 0.41 -
20 0.41 - -

BATCH MODE RESULT

Table 3.2 Calibration Curve of Conversion versus Conductivity

Ethyl Acetate Conductivity

Conversion Acetic Acid (mL)
(mL) (mS/cm)
0 100 0 0.04
0.25 75 25 0.43
0.50 50 50 0.70
0.75 25 75 0.81
1.00 0 100 0.91

5
 Table 3.3 Conversion versus conductivity

Conductivity
Time (min)
(mS/cm)
0 0.04
2 0.05
4 0.06
6 0.08
8 0.09
10 0.10
12 0.11
14 0.12
16 0.12
18 0.12

Graph of Conductivity(mS) vs Conversion(x)

1.2

1 y = 0.848x + 0.154
Conductivity,mS

0.8

0.6

0.4

0.2

0
0 0.2 0.4 0.6 0.8 1 1.2
Conversion, x

Figure 3.1 Graph conversion versus conductivity

From the figure above, the relationship between conductivity and conversion can be described
with the equation of straight line below, y is the conductivity and x is the conversion.

𝑦 = 0.848𝑥 + 0.154

6
3.2 DISUSSIONS

1. Detailed derivation of equations required to determine the rate constant (refer to main
reference as given in the following section) in batch and PBR.

The concept of rate of reaction is very important in evaluating chemical reacting systems. It is
the core factor in the development of performance models to stimulate reactor functional
parameters. Rate constant, K quantifies the speed of a chemical reaction. For a chemical
reaction where substance ethyl acetate (EtAC) and water (H2O) are reacting to produce ethanol
(EtOH) and acetic acid (HAc) the reaction rate has the form:

CH3COOC2H5 + H2O = CH3COOH + C2H5OH

r = K [CH3COOC2H5] [H2O]

Since the concentration of water (H2O) is unknown, hence it is assumed that the reaction is
first order with respect to ethyl acetate.

Table 3.4: Derivation of equation of batch and PBR

Batch reactor Packed bed reactor
Mole balance 𝑑𝑋 𝑑𝑋
𝑁𝐴0 = −𝑟𝐴 𝑉 𝐹𝐴0 = −𝑟′𝐴
𝑑𝑡 𝑑𝑊
Rate law −𝑟𝐴 = 𝐾𝐶𝐴 −𝑟′𝐴 = 𝑘′𝐶𝐴

Stoichiometry 𝐶𝐴 = 𝐶𝐴0 (1 − 𝑋)

Combine 𝑑𝑋 𝑑𝑋
𝑁𝐴0 = 𝑘𝐶𝐴0 (1 − 𝑋)𝑉 𝐹𝐴0 = 𝑘′𝐶𝐴0 (1 − 𝑋)
𝑑𝑡 𝑑𝑊
1 𝑑𝑋
𝐶𝐴0 ∫ 𝑑𝑋 = k𝐶𝐴0 ∫ 𝑑𝑡 𝐶𝐴0 𝑉 = 𝑘′𝐶𝐴0 (1 − 𝑋)
1−𝑋 𝑑𝑊

k =ln
1
×
1 𝑑𝑋 𝑘′
1−𝑋 𝑡 ∫ = ∫ 𝑑𝑊
(1 − 𝑋) 𝑉

1 1
k' = 𝑙𝑛 ×𝑉×
1−𝑋 𝑊

7
2. Using the Ergun equation to determine the bed properties. Explain why pressure drop
should not affect the conversion for liquid phase reaction.

𝑑𝑃 𝐺(1 − ∅) 150(1 − ∅)𝜇 𝑃0 𝑇 𝐹𝑇

=− [ + 1.75𝐺] ( )
𝑑𝑧 𝜌0 𝑔𝑐 𝐷𝑝 ∅3 𝐷𝑝 𝑃 𝑇0 𝐹𝑇0

Simplifying yields
𝑑𝑃 𝑃0 𝑇 𝐹𝑇
= −𝛽0 ( )
𝑑𝑧 𝑃 𝑇0 𝐹𝑇0

𝛽0 is a constant that depends only on the properties of the packed bed and the entrance
conditions.
𝐺(1 − ∅) 150(1 − ∅)𝜇
𝛽0 = [ + 1.75𝐺]
𝜌0 𝑔𝑐 𝐷𝑝 ∅3 𝐷𝑝

where
𝑃 = 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝐷𝑝 = 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑖𝑛 𝑡ℎ𝑒 𝑏𝑒𝑑 ∅ = 𝑝𝑜𝑟𝑜𝑠𝑖𝑡𝑦

𝜇 = 𝑠𝑢𝑝𝑒𝑟𝑓𝑖𝑐𝑖𝑎𝑙 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 𝑧 = 𝑙𝑒𝑛𝑔𝑡ℎ 𝑑𝑜𝑤𝑛 𝑡ℎ𝑒 𝑝𝑎𝑐𝑘𝑒𝑑 𝑏𝑒𝑑 𝑜𝑓 𝑝𝑖𝑝𝑒

𝜌 = 𝑔𝑎𝑠 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝐺 = 𝜌𝜇 = 𝑠𝑢𝑝𝑒𝑟𝑓𝑖𝑐𝑖𝑎𝑙 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦

Pressure drop does not affect the reaction rate for liquid phase reaction because liquids are
virtually incompressible and therefore the concentration does not change with pressure.
Consequently, the effect of the pressure drop on the rate of reaction can be totally ignored when
sizing liquid phase chemical reactors.

8
 3. Derive the equation to predict the conversion in the PBR. (use the specific rate constant
determined in batch mode)

Table 3.5: Batch mode PBR value

ln 1/
Time Conductivity (CEtAc/ CEtAc
(min) (mS/cm) Conductivity Conversion CEtAc0 CEtAc CHAc
CEtAc0)

0 0.04 40 0.053571 0.4 0.378571 0.021429 0.05506 2.641509

2 0.05 50 0.232143 0.4 0.307143 0.092857 0.264152 3.255814

4 0.06 60 0.410714 0.4 0.235714 0.164286 0.528844 4.242424

6 0.08 80 0.767857 0.4 0.092857 0.307143 1.460402 10.76923

8 0.09 90 0.946429 0.4 0.021429 0.378571 2.926739 46.66667

10 0.1 100 1.125 0.4 -0.05 0.45 - -20

12 0.11 110 1.303571 0.4 -0.12143 0.521429 - -8.23529

14 0.12 120 1.482143 0.4 -0.19286 0.592857 - -5.18519

16 0.12 120 1.482143 0.4 -0.19286 0.592857 - -5.18519

18 0.12 120 1.482143 0.4 -0.19286 0.592857 - -5.18519

Derivation of equation to predict conversion in PBR
1
𝐼𝑛 × 𝑣0
(1−𝑋)
k= 𝑊

1 𝑘𝑊
𝐼𝑛 =
(1 − 𝑋) 𝑣0
Final x, conversion: 0.946429
• Tubular Diameter = 8.5 cm = 0.085 m
• Tubular Radius = 4.25 cm = 0.0425 m
• Tubular Length = 42 cm = 0.42 m
• Volume, V = 𝜋 r2 L
• = 𝜋 (0.0425 m)2(0.42 m)
• = 2.383 x 10-3 m3 = 2383 mL
• Density of Amberlyst 131= 0.0375 g/mL (M.B. Taysun et al.)
• Weight of catalyst used= Density of catalyst × Volume of reactor
0.0375𝑔
• 𝑊= × 2383𝑚𝐿 = 89.3625𝑔𝑐𝑎𝑡
𝑚𝐿

9
Rate constant in batch reactor:

k= 0.655 mL/min.gcat

4) Using the equation derived in step 3 and using the experimental conversion data,
determine the rate constant at different flow rates. Compare the specific rate constants
and analyse the deviations.

Table 3.6: PBR conversion value in different flowrates

Flow Rate
20 30 40 20 30 40
(mL/min)
Conductivity of the efficient at outlet
Time (min) conversion
(mS/cm)
0 - - - - - -
88.9411 37.1764 32.4705
2 0.91 0.47 0.43
8 7 9
80.7058 27.7647
4 0.84 0.46 0.39 36
8 1
73.6470 34.8235 26.5882
6 0.78 0.45 0.38
6 3 4
64.2352 33.6470 25.4117
8 0.7 0.44 0.37
9 6 6
59.5294 32.4705 25.4117
10 0.66 0.43 0.37
1 9 6
46.5882 31.2941 25.4117
12 0.55 0.42 0.37
4 2 6
37.1764 30.1176
14 0.47 0.41 - -
7 5
30.1176 30.1176
16 0.41 0.41 - -
5 5
30.1176 30.1176
18 0.41 0.41 - -
5 5
30.1176
20 0.41 - - -
5

Rate constant for PBR:

1
𝐼𝑛 × 𝑣0
(1−𝑋)
Equation of Rate constant PBR, k = 𝑊

Table 3.7: Rate constants summary in different flowrates

Volumetric flowrate, 𝒗𝟎 20 mL/min 30 mL/min 40 mL/min

Conversion, X 0.301176 0.301176 0.254117

10
 Weight of catalyst, W 89.3625 gcat
Rate constant PBR, k
0.08 0.12 0.13
(mL/min.gcat)

5. Comparison of results obtained with the experimental data reported in the literature
for similar conditions.

The rate constant of the batch reactor is 0.0085 min-1, which is obtained from the slope of
Figure 2. On the other hand, the rate constants of PBR at 20 mL/min, 30 mL/min and 40
mL/min are 0.08 mL/min.gcat, 0.12 mL/min.gcat and 0.13 mL/min.gcat respectively.

According to Affum, in PBR, the rate constants will increase when the flowrates
increase. From the results, the values of rate constant are 0.08 mL/min.gcat, 0.12 mL/min.gcat
and 0.13 mL/min.gcat for 20mL/min, 30mL/min and 40mL/min repectively. The flow rates of
the reactants is proportional to the reaction rate constant based on the formula for derivation of
1
𝑣0 𝐼𝑛
(1−𝑋)
rate constant in PBR, k = . It has been aided by the larger gradient in (1 – x), with the
𝑊

conversion, x becoming a smaller value.

However, reaction rate constant should be constant under the same temperature
theoretically. The reaction rate constants change because hydrolysis is an endothermic reaction,
and the value of reaction rate constants depend on the temperature, therefore the values of the
reaction rate constants vary. Reaction rate constants also depend on the presence of a catalyst
and in gas-phase reactions, it may be a function of total pressure (Fogler, 2006). Hence, the
experimental result followed the theory except at flowrate of 20 mL/min and almost constant
as the flowrates increase.

6. Comments on the differences in the results obtained and discussion of the results and
the quality of the data and experimental procedures (difficulties and uncertainties).

Condition in packed bed reactor such as undesired thermal gradients might exist, the
temperature control is poor, channeling may occur and the difficulty may occur during unit
service and cleaning affect the result of the performances.

11
4.0 CONCLUSION AND RECOMMENDATIONS

In this experiment, we are aimed to determine the reaction rate constant for the acid-
catalysed liquid-phase hydrolysis of ethyl acetate (EtAc) to ethanol (EtOH) and acetic acid
(HAc) in batch and packed bed reactor (PBR). From our experimental data for batch mode, we
found out that this reaction is a second order reaction with a rate constant of 0.655 mL/min.gcat
by using integral method to analyse the concentration-time data. For PBR, we obtained
different rate constant for different feed flow rate via tedious calculation using experimental
conversion data. For the flow rate of 20mL/min, the rate constants is 0.08 mL/min.gcat while
for the flow rate of 30mL/min, the rate constant is 0.12 mL/min.gcat. The rate constant is 0.13
mL/min.gcat for a feed flow rate of 40 mL/min. From this result, we can conclude that the
lower the feed flow rate, the lower the retention time of the reactant inside the reactor, the lower
the rate constant. The higher the rate of reaction, the lower of conversion can be achieved.

As recommendation, we recommend that the apparatus that used for this experiment
such as volumetric flask, measuring cylinders, dropper and pail should be clean well to prevent
any contamination that would create the result error. Before conducting the experiment, we
suggest that all the liquids should be drained off from the unit. Then, the feed tanks should be
rinsed with clean water and filled with deionized water to ensure the accuracy of the
experimental data. Before the calibration, the conductivity meter should be rinsed with standard
solution so that the reading will not affect by previous experiment. The solution must exceed
the hole of conductivity meter that immersed into the solution when measuring the
conductivity. During the experiment, the solution must be allowed to flow long enough to let
the reactor achieve steady state. Apart from that, all the valve must be closed to avoid spillage
that will affect the results.

12
5.0 REFERENCES

1. Fogler, H. (2006). Elements of Chemical Reaction Engineering. 4th ed. U.S: Pearson,
pp.871-895.
2. University of Michigan (2015). Collection and Analysis of Rate Data. Retrieved from
http://www.umich.edu/~elements/fogler&gurmen/html/course/lectures/five/index.htm
3. University of Michigan (2015). Conversion and Reactor Sizing. Retrieved from
http://www.umich.edu/~elements/fogler&gurmen/html/course/lectures/two/index.htm

13
6.0 APPENDICES

Figure 6.1: PBR operator data

14
 BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 5

THE ENZYMATIC SYNTHESIS OF ETHYL BUTANOATE BY USING

IMMOBILISED LIPASE

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID

1 RADHWA BINTI MUHAMMAD FARID KA17204

2 VINODHINI A/P JAYASEELAN KA17094

3 NUR FARISAH BINTI AKMAL KA17161

4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273

5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS & DISCUSSIONS 5

4.0 CONCLUSION AND RECOMMENDATION 11

5.0 REFERENCES 12

6.0 APPENDICES 13

2
1.0 ABSTRACT

Response surface methodology was used to determine optimum conditions for the
esterification of ethanol and butyric acid to produce a flavor ester using immobilized lipase
by Candida Antarctica. The objective of this study was to investigate the potential of the ester
production using different feedstock and catalyst. Various reaction parameters including acid
and alcohol concentration, enzyme concentration, temperature and reaction time affecting the
synthesis of ethyl butyrate were investigated. The experiment was start by dissolving 2g of
NaOH into 500 mL of distilled water and was put in the burette for titration purposes.
Phenolphthalein is dissolved in 50 mL Butanol and 50 mL distilled water. Then 28.96 mL of
Acetic Acid is measured and mix with 470 mL of distilled water to produce 500 mL of 1.0 M
of Butanol solution. Next, 46 mL of Butanol is mixed with distilled water until get the 500
mL volume which produce 1.0 M Butanol. 100 mL of butanol solution and 100 mL of Acetic
Acid solution is mixed and 0.4g of lipase was added. The solution was then be heated at
temperature of 35ºC at 4rpm. 5 mL sample was taken for every 2 minutes interval. 4 drops of
Phenolphthalein was added to the sample and titrated with NaOH solution. This experiment
was repeated at 45ºC. The principal parameters influencing the esterification yield were the
temperature and substrate concentration. The result shows decrease in the volume of NaOH
required as the time passed by. The results indicated that when optimal 10.87 M butanol and
17.45 M acetic acid were catalyzed by the immobilized lipase at 35ºC, the highest conversion
yield of 14% were obtained while for 45ºC, the highest conversion yield were 20%. This is a
kinetic model of Ping Pong Bi-Bi mode with inhibition of both substrates was proposed and
validated by experimental data. In order to obtain a higher mass transfer coefficient, the
particle size must be small enough (if the real reaction rate needs to be very small) to have a
reaction-limited reaction. Hence, the size of lipase is suitable when it small.

3
2.0 METHODOLOGY

(A) Preparation of Phenolphthalein Solution:

1g of the phenolphthalein 10 mL of water is added to the beaker

powder is weighed and after the phenolphthalein powder is
dissolved in 50 mL of butanol dissolved completely in the butanol.
in a beaker.

(B) Preparation of NaOH Solution:

2 g of NaOH is weighed and then

dissolved in 500 mL of distilled 0.1 M NaOH solution is filled into
water to form 500 mL of 0.1 M of a burette for titration purpose.
NaOH solution.

(C) Experimental Procedure:

The mixture is titrated

0.5 g of enzyme 4 drops of with NaOH solution until a
lipase is measured phenolphthalein pink colour appears. The
and prepared. solution are added to volume of NaOH needed is
the conical flask recorded. The extraction
containing 1.0 mL of process is repeated until
extracted solution. the volume of NaOH
needed becomes constant.
28.96 mL of acetic
acid is measured and
diluted with distilled For every two minutes of
water up to 500 mL to interval, 1.0 mL of solution
form 1.0 M of acetic inside the beaker is extracted The experiment is
acid solution. by using 1 mL pipette into a repeated at the
conical flask. temperature of 35 ºC of
mixture solution.

46 mL of butanol is Then, 50 mL of each

measured and diluted solutions respectively is
with distilled water up measured and mixed
to 500 mL to form 1 M together with 0.5g of lipase
of butanol solution. and poured into a beaker.
4
 Temperature (oC) 35 oC 45 oC

Time (min)
3.0 RESULTS AND DISCUSSIONS

RESULT :

Table 3.1: Preparation of Solution for Experiment

For 200 mL of 1.5 M of Butanol solution: For 200 mL of 1 M of Acetic Acid

solution:
• MW of Butanol = 74.12 g/mol
• Density = 810 g/L • MW of Acetic Acid = 60.05 g/mol
• Purity = 99.5 % • Density = 1050 g/L
• Purity = 99.8 %
Molarity of Butanol
Molarity of Acetic Acid
𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 𝐷𝑒𝑛𝑠𝑖𝑡𝑦
= 𝑀𝑊 𝑃𝑢𝑟𝑖𝑡𝑦 𝑥 𝐷𝑒𝑛𝑠𝑖𝑡𝑦
=
0.995 𝑥 810 𝑔/𝐿 𝑀𝑊
= 74.12 𝑔/𝑚𝑜𝑙 0.998 𝑥 1050 𝑔/𝐿
= 60.05 𝑔/𝑚𝑜𝑙
= 10.87 M
= 17.45 M

Dilution:
Dilution:
M1V1 = M2V2
M1V1 = M2V2
(10.87 M) V1= (1.5 M) (200 mL)
(17.45 M) V1 = (1 M) (200 mL)
V1 = 27.6 mL
V1 = 11.46 mL

For 500 mL of 0.1 M Sodium Hydroxide solution:

• Molar mass of sodium hydroxide = 40 g/mol

𝑁𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒
Molarity = 𝑉𝑜𝑙𝑢𝑚𝑒 Mass required = No. of mole x Molar mass

No. of mole = Molarity x Volume = 0.02 mol x 40 g/mol

= 0.1 mol/L x 0.2 L = 0.8 g

= 0.02 mol

Weight of lipase used:

Weight of lipase used = 0.4 g

5
 35 oC 45 oC

Temperature (oC) Volume of NaOH required (mL)

0 0 0

2 25 25

4 25 24.5

6 24 24.2

8 23.7 23.7

10 23.4 23.2

12 22.6 23

14 22.4 22.5

16 21.8 20

18 21.6 20

20 21.5 20

22 21.5 20

24 21.5 20

6
 Volume of titrant, 0.1M NaOH
required versus time 37'C & 40'C
Volume of NaOH required (mL) 30
25
20
15
35 'C
10
45'C
5
0
0 5 10 15 20 25 30
Time (min)

Figure 3.1: Volume of titrant, 0.1 M NaOH required versus time 35℃ & 45℃

Conversion (%) =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑎𝑡 𝑡=0−𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑎𝑡 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑡𝑖𝑚𝑒
𝑥 100%
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑎𝑡 𝑡=0𝑠

Assumptions: 1) Concentration change is very small and negligible after 1 ml of solution is

withdrawn.

2) Concentration of acetic acid in the mixed solution after withdrawal of 1ml

solution at each interval is the same as the concentration of acetic acid in the
mixed solution before withdrawal of 1ml solution

3) Volume of NaOH requirEd at specific time corresponds to the

concentration of acetic acid at the specific time.

Table 3.2: Conversion of reaction versus time at 35 ℃ & 45 ℃

Temperature 35oC 45oC

(oC) Volume of Conversion Volume of Conversion

NaOH NaOH

7
Time (min)

0 0 0 0 0

2 25 25 − 25 25 25 − 25
𝑥 100% 𝑥 100%
25 25
= 0% = 0%

4 25 25 − 25 24.5 25 − 24.5
𝑥 100% 𝑥 100%
25 25
= 0% = 2%

6 24 25 − 24 24.2 25 − 24.2
𝑥 100% 𝑥 100%
25 25
= 4% = 3.2%

8 23.7 25 − 23.7 23.7 25 − 23.7

𝑥 100% 𝑥 100%
25 25
= 5.2% = 5.2%

10 23.4 25 − 23.4 23.2 25 − 23.2

𝑥 100% 𝑥 100%
25 25
= 6.4% = 7.2%

12 22.6 25 − 22.6 23 25 − 23
𝑥 100% 𝑥 100%
25 25
= 9.6% = 8%

14 22.4 25 − 22.4 22.5 25 − 22.5

𝑥 100% 𝑥 100%
25 25
= 10.4% = 10%

16 21.8 25 − 21.8 20 25 − 20
𝑥 100% 𝑥 100%
25 25
= 12.8% = 20%

18 21.6 25 − 21.6 20 25 − 20
𝑥 100% 𝑥 100%
25 25
= 13.6% = 20%

20 21.5 25 − 21.5 20 25 − 20
𝑥 100% 𝑥 100%
25 25
= 14% = 20%

22 21.5 25 − 21.5 20 25 − 20
𝑥 100% 𝑥 100%
25 25
= 14% = 20%

24 21.5 25 − 21.5 20 25 − 20
𝑥 100% 𝑥 100%
25 25
= 14% = 20%

8
 Conversion of reaction versus time at
35'C, 45'C
Conversion of reaction (%) 25

20

15

10 35oC

5 45oC

0
0 5 10 15 20 25 30
-5
Time (min)

Figure 3.1: Conversion of reaction versus time at 35℃ & 45 ℃

DISCUSSIONS

1. What is the offset to eliminate the mass transfer effect of the immobilized lipase in the
reaction kinetic study?

According to the article (Yadav and Trivedi, 2003), in immobilized-enzyme catalyzed

reactions, the magnitudes of external mass transfer resistance and intra-particle diffusion
limitation play a crucial role and affect intrinsic kinetics. By the speed of agitation, the offset
to remove the mass transfer effect of the immobilized lipase in the reaction occurs. 4 rpm was
set as the speed for the magnetic stirrer in this experiment. Compared to the volume of the
solution used, which is very small and about 100 mL, it is considerably large and the quantity
of lipase used is just 0.4 g. The small size of the heterogeneous immobilized lipase region in
the reaction kinetic analysis also helps to eliminate the mass transfer effect of the
immobilized lipase. The coefficient of mass transfer, kc, is inversely proportional to the
square root of particle size, according to Fogler (2014). In order to obtain a high mass transfer
coefficient, if the real reaction rate needs to be very small, the particle size must be small
enough to have a reaction-limited reaction. Hence, the size of lipase must be small.

9
2. How the limiting reactant is measured?

In a chemical reaction, the controlling reactant is the reactant that restricts the amount of
product that can be produced or the amount of reactant that will be used first. The reaction
will end when all the limiting reactant has been used up, and no further reaction will occur
and we can consider when the reaction is complete. In this experiment, acetic acid was
determined as the limiting reactant because the higher concentration of acetic acid could
damage the enzyme's hydrolytic layer structure causing lipase deactivation. Through the
volume of 0.1M NaOH required for titration, the conversion of reaction, X can be
determined.

3. What rate law is used to elaborate the kinetics of the esterification reaction?

In the absence of any intra-particle diffusion limitations, the kinetics of liquid phase reactions
catalysed by ion exchange resin are usually modelled by PseudoHomogeneous (PH) or
Langmuir-Hinshelwood (LHW) models (Gangadwala et. al., 2003; Chakrabarty and Sharma,
1993). In this case, for small amounts of water in the reactor, the pseudo homogeneous model
is adequate and the objective of the experiment was the kinetic against time rather than
catalyst weight used due to the type of reactor.

10
4.0 CONCLUSION AND RECOMMENDATION

In conclusion, the amount of sodium hydroxide (NaOH) has been used in the
esterification of acetic acid and butanol using immobilized lipase to determine the
temperature relationship on the kinematic enzymatic synthesis of butyl acetate. In the
reaction mixture NaOH is able to neutralize the acid. The amount of NaOH required in 35℃
is higher than 45℃ from the results. However, the time taken to hold the NaOH volume
constant at 45℃ is less than the 35℃ temperature. Finally, it fits the Theory of Le Chatelier.
The theory of the Chatelier increases the temperature of a system which favors the
endothermic reaction. Therefore, the reaction rate increases as the temperature increases in
this experiment.

Any suggestions to enhance the outcome of this experiment are proposed. Before the
mixture gets heated, first, prepare the phenolphthalein. All the equipment, including dropper,
beaker, conical flask and burette should be cleaned before the experiment is performed. This
means that the substance is not contaminated. After the NaOH must be titrated in the conical
flask in the drop-by-side direction to change the solution's light-pink color. Finally, to make
sure that the reactions react more quickly, we suggest that the enzyme mass be increased.

11
5.0 REFERENCES

1. Tmatovic. (2015, October 7). SPR Tips: 3 Ways To Limit Mass Transfer Effects In Kinetic
Data. Retrieved September 25, 2017, from nicoya LIFESCIENCES:
https://nicoyalife.com/blog/3-ways-to-limit-mass-transfer-effects/

2. Sarick Shah.(2020, August 16). Limiting Reagent Retrieved from:

https://batch.libretexts.org/print/url=https://chem.libretexts.org/Bookshelves/Inorganic_Chemistr
y/Modules_and_Websites_(Inorganic_Chemistry)/Chemical_Reactions/Limiting_Reagents.pdf

12
6.0 APPENDICES

Figure 6.1: Results of Bioreactor

13
 BKF3741 CHEMICAL REACTION ENGINEERING LAB

SEMESTER 1 2020/2021

EXPERIMENT 6

RESIDENCE TIME DISTRIBUTION ANALYSIS OF A CONTINUOUS STIRRED

TANK REACTOR

INSTRUCTOR’S NAME : DR RUZINAH BINTI ISHA

SECTION : 04

GROUP NO. : 02

NO. NAME ID
1 RADHWA BINTI MUHAMMAD FARID KA17204
2 VINODHINI A/P JAYASEELAN KA17094
3 NUR FARISAH BINTI AKMAL KA17161
4 KHALED NASSER ABDULLAH ABDO AL-GAFRI KA16273
5 DURA AMIRA BINTI NOOR AZMI KA18221

1
 TABLE OF CONTENT

NO. CONTENT PAGE

1.0 ABSTRACT 3

2.0 METHODOLOGY 4

3.0 RESULTS & DISCUSSIONS 5

4.0 CONCLUSION AND RECOMMENDATION 10

5.0 REFERENCES 11

6.0 APPENDICES 12

2
2.0 METHODOLOGY

1. Preparation of calibration curve

A series of different salt concentrations was prepared by diluted it with deionized

water.

The response factor from the conductivity meter was obtained.

2. Experimental procedure

The valves (V6 and V7) is

The experimental set up was adjusted so that the water from
shown in the module figure. T2 only flows to CT3. Discharge
Water was added at Tank T2
Vessel CT3 is used for the RTD valve is adjusted to “open”
study. while the sampling valve is
adjusted to “closed”.

Pump 2 is started and the

rotameter V2 is adjusted to the 5.0 g of table salt was
maximum reading to fill up the Pump 2 was turned off upon transfered into CT3. The stirrer
CT3 until it overflows. The steady flow was attained. was started and stirring speed
volume of CT3 at overflow was kept at 200 rpm.
condition was about 1500 mL.

The conductivity meter

The rotameter V2 was turned
(Conductivity Controller 4 on The conductivity reading at
on and the flow is adjusted to
the control panel) was being every 2 minutes interval for at
150 ml/ min and the timer was
monitored until it reached least 30 minutes was obtained.
started.
constant value.

3. Shutdown Procedure

All liquids were

After the experiment Any spillage from the
disposed immediately
was complete, all unit were wipe off
after each experiment.
liquids were drained immediately. Then,
Any solution or waste
off from the reactor the reactor was
in the tanks cannot be
and the reactor were flushed with water for
left over a long period
cleaned properly. 2 times.
of time.

3
3.0 RESULTS AND DISCUSSIONS
3.1 RESULTS
Table 3.1: Data Required for Calibration Curve
Weight (g) Concentration of NaCl (mol/L) Conductivity (mS/cm)

0 0 0.08
0.5 0.005704 0.72
1.0 0.0114 1.33
1.5 0.0171 1.88
2.0 0.0228 2.51
2.5 0.0285 3.27
3.0 0.0342 3.67
3.5 0.0399 4.39
4.0 0.0456 4.88
4.5 0.0513 5.45
5.0 0.0570 6.11

Conductivity vs Concentration
7
y = 105.11x + 0.1217
6
R² = 0.999
Conductivity (mS/cm)

0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration (mol/L)

Figure 3.1: Calibration Curve of Conductivity vs Concentration

From the calibration curve, the equation retrieved is y = 105.11x + 0.1217 with y
represents conductivity and x represents concentration of solutions. In order to find the
concentration from conductivity, x = (y-0.1217)/105.11.

4
3.2 DISCUSSION

1. Plot the transient concentration profile.

Table 3.2: Data of Conductivity and Concentration of Table Salt Solution with Respect to Time
Time (min) Concentration of NaCl (mol/L) Conductivity (mS/cm)

0 0.0573 6.14
2 0.0466 5.02
4 0.0359 3.90
6 0.0291 3.18
8 0.0236 2.60
10 0.0193 2.15
12 0.0153 1.73
14 0.0122 1.40
16 0.009498 1.12
18 0.007309 0.89
20 0.005026 0.65
22 0.003980 0.54
24 0.003137 0.47
26 0.003028 0.44
28 0.002648 0.40
30 0.002077 0.34
32 0.001887 0.32
34 0.001601 0.29
36 0.001601 0.29
38 0.000840 0.21
40 0.000840 0.21
42 0.000840 0.21
44 0.000555 0.18
46 0.000364 0.16
48 0.000174 0.14
50 -0.000016 0.12
52 -0.000206 0.10
54 -0.000302 0.09
56 -0.000302 0.09
58 -0.000302 0.09
60 -0.000302 0.09

5
 Concentration of NaCl vs Time
0.07

0.06

0.05
Concentration (mol/L)

0.04

0.03

0.02

0.01

0
0 10 20 30 40 50 60 70
-0.01
Time (min)

Figure 3.2: Graph Concentration of NaCl against Time

Using the equation obtained from the calibration curve, conductivity can be converted
to concentration and the transient concentration profile can be plotted as seen in Figure 3.2.
The concentration dropped as the time increased on the basis of the graph. This is because time
for atoms in the reactor is different and the distribution of different atoms in the reactor is
different in terms of the time which is called the RTD (Residence Time Distribution). The
longer the time, the longer the RTD, the lower the salt ions used for the experiment as tracer
remaining in the reactor. Moreover, as the time increased, more Na+ and Cl ions attracted water
molecules. Conductivity and concentration therefore decrease as time increases, so the reactor
has kept less free ions.

2. Determine the RTD parameters based on the collected data.

Based on the result collected, the residence-time distribution (RTD) function, E(t) can be
determined using this formula :

𝐶(𝑡)
𝐸(𝑡) = 60
∫0 𝐶(𝑡)𝑑𝑡

6
 To obtain E(t) curve from the C(t) curve, we just divide C(t) by the integral ∫ C(t)dt ∞
0 which is the area under the C curve, then we calculate the area under curve by using
Simpson’s 3/8 rule.

Table 3.3: Simpson’s 3/8 rule

Time (min) Simpson’s 3/8 rule

0–6 0.18782
6 – 12 0.09737
12 – 18 0.04933
18 – 24 0.02107
24 – 30 0.01251
30 – 36 0.00795
36 – 42 0.00421
42 – 48 0.00212
48 – 54 -0.000447
54 – 60 -0.001359

60

∫ 𝐶(𝑡)𝑑𝑡 = 0.380574
0

Table 3.4: Data of Conductivity, Concentration of Salt Solutions, and Residence Time Distribution
Function, E(t) with its respective time.

Time Concentration (mol/L) Conductivity (mS/cm) Residence Time

(min) Distribution, E(t)
(l/min)
0 0.0573 6.14 0.150562
2 0.0466 5.02 0.122447
4 0.0359 3.90 0.094331
6 0.0291 3.18 0.076463
8 0.0236 2.60 0.062012
10 0.0193 2.15 0.050713
12 0.0153 1.73 0.040202
14 0.0122 1.40 0.032057
16 0.009498 1.12 0.024957
18 0.007309 0.89 0.019205
20 0.005026 0.65 0.013206
22 0.003980 0.54 0.010458
24 0.003137 0.47 0.008243

7
26 0.003028 0.44 0.007956
28 0.002648 0.40 0.006958
30 0.002077 0.34 0.005458
32 0.001887 0.32 0.004958
34 0.001601 0.29 0.004207
36 0.001601 0.29 0.004207
38 0.000840 0.21 0.002207
40 0.000840 0.21 0.002207
42 0.000840 0.21 0.002207
44 0.000555 0.18 0.001458
46 0.000364 0.16 0.000956
48 0.000174 0.14 0.000457
50 -0.000016 0.12 -4.2E-05
52 -0.000206 0.10 -0.00054
54 -0.000302 0.09 -0.00079
56 -0.000302 0.09 -0.00079
58 -0.000302 0.09 -0.00079
60 -0.000302 0.09 -0.00079

Graph of E(t) vs Time

0.16
0.14
0.12
0.1
0.08
E(t)

0.06
0.04
0.02
0
-0.02 0 10 20 30 40 50 60 70
y = -0.0017x + 0.0744
-0.04
Time

Figure 3.3: Graph of E(t) vs Time

8
3. From the trend of RTD, suggest prevailing issues. Determine whether the reactor is
an ideal CSTR?

The residence time distribution (RTD) of a chemical reactor is a probability distribution

function that describes the amount of time a fluid element could spend inside the reactor.
Residence time Distribution (RTD) is a useful diagnostic tool to characterize the mixing and
flow within reactors and to compare the behaviour of real reactors to their ideal models. In an
ideal continuous stirred-tank reactor (CSTR), the flow at the inlet is completely and instantly
mixed into the bulk of the reactor. The reactor and the outlet fluid have identical, homogeneous
compositions at all time (Nauman, E. Bruce). Besides, according to Werner at el, the graph
should produce a narrow peak and moves closer to unity afterwards if it is an ideal CSTR. From
Figure 3.3, we can observe that the E(t) decreases with the time. So, since our graph shows an
exponential curve, we can assume that the reactor is not an ideal CSTR. The CSTR non- ideality
is probably because there is a less effective mixing regime. However, this situation can be
overcome by increasing the stirrer speed, decreasing the solution viscosity or more effective
reactor baffling. (Yung and Paula, 1995).

9
4.0 CONCLUSIONS AND RECOMMENDATION

It can be concluded that the conductivity of the solution decreased and achieved
constant throughout the reaction time. This is due to the solution is being diluted with the pure
water. In the other hand, the conversion also decreased as time passed. The graph plotted shows
that conductivity decreases from 6.14 mS/cm to 0.09m S/cm within 54 minutes time frame and
become constant until time reached 60 minutes. This also shows that the concentration is
inversely proportional to time. From the trend of RTD obtained, the existed CSTR reactor is
not performed as an ideal condition where we obtain an exponential graph.

To increase the precision and safety of the experiment, make sure that the conductivity
metre is well calibrated before it is used to decrease the instrumentation error for the
recommendations. In addition, the conductivity metre must also be rinsed with water after each
reading has been taken. Furthermore, to extract (wash) and flash out the impurity that could
lead to the conductivity reading, the reactor must first be purged with pure water. In addition,
the CSTR water pump was not smooth, allowing the tracer to flow out at a higher rate, and the
flow rate is not constant. Thus, by changing the value of the flow rate, the flow rate must be
kept the same during the experiment. Finally, the stirring speed must be increased and the
solution viscosity should be reduced in order for the CSTR reactor to operate in a nearly perfect
and optimal state.

10
5.0 REFERENCES

1. Nauman, E. Bruce (May 2008). "Residence Time Theory". Industrial & Engineering
Chemistry Research. 47 (10): 3752–3766.

2. C.W.Yung & Paula A. Berezansky. (1995). Low Electrolytic Conductivity Standards

521. Journal of Research of the National Institute of Standards and Technology, 100,
521-527

3. Chaplin, M. (6 August, 2014). Continuos Flow Stirred Tank Reactor. Retrieved from
Enzyme technology: http://www1.lsbu.ac.uk/water/enztech/cstr.html

4. Fogler, H. (2008). Distribution of residence times for chemical reactors. In H. Fogler,

Elements of Chemical Reaction (p. 867). Pearson.

5. Smart Fertilizer Management. (4 September, 2015). Retrieved from Smart Library:

https://www.smart-fertilizer.com/articles/electrical-conductivity

11
6.0 APPENDICES

Figure 6.1: Results of CSTR-RTD

12