TABLE OF CONTENT

TITLE

PAGES

Abstract / Summary

Introduction

Objectives

Theory

Apparatus

Procedures

Results

11

Sample calculation

14

Discussion

17

Conclusion

19

Recommendation

20

Reference

21

Appendix

22

ABSTRACT
Reactors are used in the chemical industry for the millions of processes. One of
many different types of reactors is plug flow reactor (PFR). A plug flow reactor is a pipe1

shaped tank where a chemical reaction takes place with walls coated with a catalyst and an
inlet flow of pure reactant. The plug flow reactor (PFR) is used in this experiment. There
are a few of objectives that are needed to achieved in this experiment such as to find out
the calibration curve of conversion of sodium hydroxide, NaOH versus conductivity, to
carry out a saponification reaction between NaOH and Et(Ac) in a PFR, and to determine
the rate of reaction, rate law, and the reaction rate constant. Besides that, this experiment
also wants to determine the conversion of NaOH in the reactor and the effect of residence
time on the conversion in a PFR. There are few of graph being plotted with the results that
are got from the experiment. One of them is the graph conductivity versus conversion for
experiment 1. This graph that had being plotted is inversely proportional. Next graph is
plotted between conversions of NaOH in reactor versus residence time distribution. This
shows that the residence time is increased as the conversion of NaOH increased. The rate
of reaction and rate constant can be calculated after know the values of conversions.
However, the value of conversion in this experiment is exceed 100% and this affect the
value of rate of reaction.

INTRODUCTION

Reactors are used in the chemical industry for the millions of processes. There are
2

many different types of reactors due to many different factors that can control the
formation of product during the reaction. One of many different types of reactors is plug
flow reactor (PFR).

A plug flow reactor is a pipe-shaped tank where a chemical reaction takes place
with walls coated with a catalyst and an inlet flow of pure reactant 1. The plug flow reactor
has an inlet flow composed of the reactants. The reactant flow into the reactor and is the
converted into the product by certain chemical reaction. The product flows out of the
reactor through the outlet flow. In many scenarios, a catalyst is involved in the reaction.
Figure below shows that how the enzyme coats the interior of the wall.

Furthermore, plug flow reactors are an idealized scenario where is no mixing

involved in the reactor. Since PFR is an idealized reactor, it does not truly exist in the real
world. It is impossible to have no mixing at all during a reaction, but the amount of mixing
in the reactor can minimize.

Plug flow reactors are frequently used in the chemical industry due to the nonmixing property of the reactors. Plug flow reactors are frequently used in biological
reactions when the substrate flows into the reactor and is converted to product with the
use of an enzyme. Besides that, plug flow reactor are useful for continuous production
because they have an inlet and outlet stream. In a conclusion, plug flow reactors are most
useful for continuous production, large-scale reactions, or fast reactions.

1 Plug Flow Reactor, Product Description by Matthew Grisewood (http://www.scribd.com/doc/29195386/Plug-Flow-Reactor)

3

OBJECTIVE

Experiment 1:
1. To find the calibration curve of conversion versus conductivity.

Experiment 2 and 3:

1. To carry out a saponification reaction between NaOH and Et(Ac) in a plug flow
reactor (PFR).

2. To determine the rate of reaction, rate law, and raction rate constant.
3. To determine the conversion of NaOH in the reactor.
4. To determine the effect of residence time on the conversion in a plug flow reactor
(PFR).

THEORY
5

Conversion
The conversion, XA is the number of moles of reactant that have reacted per mole of
reactant fed to the system.
XA =

moles of reactant reacted

moles of reactant fed

Residence time,
The residence time distribution (RTD) of a reactor is a characteristic of the mixing that
occurs in the chemical reactor.
Residence time, =
where:

V PFR
V0

V PFR
V0

= reactor volume
= total feed flow rates

Rate Of Reaction And Rate Law

The reaction rate (rate of reaction) or speed of reaction for a reactant or product in a
particular reaction is intuitively defined as how fast or slow a reaction takes place 2. For
simple definition, the rate of reaction, -r A, is the number of moles of reactant reacting
(disappearance) per unit time per unit volume (mol/dm3.s)3.
The reaction rate equation (or the rate law) is essentially an algebraic equation involving
concentration. The common general forms of the rate law equation is shown,
-rA = kACACA
where CA and CB are the individual reactants concentrations, each raised to the powers
and , while kA is the reaction rate constant.
The order of the reaction refers to the powers to which concentrations are raised in the
2 http://en.wikipedia.org/wiki/Plug_flow_reactor_model
3 H. Scott Fogler, Elements of Chemical Reaction Engineering, 4th Edition, Pearson International Edition (2006)
6

reaction rate law. From equation above, the overall order of the reaction, n is,
n=+
For this experiment, this reaction is a second order equimolar with the same initial
reactant concentration (CAo = CBo), the rate law shown to be:

where:

= extent of conversion

CA

= exit concentration of reactant NaOH [M]

VO

= total inlet flowrate of solutions (mL/min)

CAo

= inlet concentration of reactant NaOH in the reactor [M]

The reaction rate constant can be determined by:

k

Vo
X
V PFR C Ao 1X

APPARATUS AND MATERIALS

APPARATUS:

Beaker

Conical flask

Burette

Plug flow reactor (Model: BP 101)

Conductivity meter

Measuring cylinder

MATERIAL:

Sodium hydroxide solution, NaOH (0.1M)

Sodium acetate solution, Na (Ac) (0.1M)

Deionised water, H2O

Hydrochloric acid solution, HCl (0.25M)

PROCEDURES

EXPERIMENT 1

Preparation of calibration curve for conversion versus conductivity

1. The following solutions were prepared:

1 liter of sodium hydroxide, NaOH (0.1M)

1 liter of sodium acetate, Na(Ac) (0.1M)

1 liter of deionised water, H2O

2. The conductivity and NaOH concentration for each conversion values was
determined by mixing the following solutions into 100 ml of deionised water:

0% conversion

: 100 ml NaOH

25% conversion

: 75 ml NaOH + 25 ml Na(Ac)

50% conversion

: 50 ml NaOH + 50 ml Na(Ac)

75% conversion

: 25 ml NaOH + 75 ml Na(Ac)

100% conversion

: 100 ml Na(Ac)

3. All data were recorded.

4. The calibration curve of conductivity versus conversion was plotted. The slope and
y-axis intercept was determined.

EXPERIMENT 2

Effect of residence time on the reaction in a TFR

1. The general start-up procedures were performed.
2. Valves V9 and V11 were opened.
3. Both the NaOH and Et(Ac) solutions were allowed to enter the plug reactor R1 and
empty into the waste tank B3.
4. P1 and P2 were adjusted to give a constant flow rate of about 300 ml/min at flow
meters FI-01 and FI-02. Make sure that both flow rates are the same. The flow rates
were recorded.
5. The inlet (QI-01) and outlet (QI-02) conductivity values were started monitored
until they do not change over time. This is to ensure that the reactor has reached
steady state.
6. Both inlet and outlet steady state conductivity values were recorded. The
concentration of NaOH exiting the reactor and extent of conversion from the
calibration curve were found.
7. Sampling valve V15 was opened and a 50ml sample was collected. A back titration
procedure was carried out to manually determine the concentration of NaOH in the
reactor and extent of conversion.
8. Step 4 to 7 were repeated for different residence times by reducing the feed flow
rates of NaOH and Et(Ac) to about 250, 200, 150, 100 and 50 ml/min. make sure that
both flow rates are the same.
10

EXPERIMENT 3

Back titration procedures for manual conversion determination

1. A burette was filled up with 0.1M NaOH solution.
2. 10 ml of 0.25M HCl was measured in a flask.
3. 50 ml sample was obtained from the experiment and the sample was added to the
HCl immediately in the flask to quench the saponification reaction.
4. A few drops of pH indicator were added into the mixture.
5. The mixture was titrated with NaOH solution from the burette until the mixture is
neutralized. The amount of NaOH titrated was recorded.

RESULTS
Experiment 1:

SOLUTION MIXTURES

CONVERSION

CONDUCTIVITY

0.1 M

0.1 M

H2O

(%)

(mS)

NaOH
100 mL
75 mL
50 mL
25 mL
-

Na(Ac)
25 mL
50 mL
75 mL
100 mL

100 mL
100 mL
100 mL
100 mL
100 mL

0
25
50
75
100

12.46
10.46
8.72
6.50
4.66

11

CONDUCTIVITY versus CONVERSION

14
12

f(x) = - 0.08x + 12.47

10
8
CONDUCTIVITY (mS)

6
4
2
0
0

20

40

60

80

100

120

CONVERSION (%)

12

Experiment 2:

Reactor volume

= 0.4 L

Concentration of NaOH in the feed tank

= 0.1 M

Concentration of Et(Ac) in the feed tank

= 0.1 M

FLOW
NO

1
2
3
4
5
6

FLOW

RATE OF RATE OF

OUTLET

TOTAL FLOW
RATE OF

RESIDENCE
TIME (min)

NaOH

Et(Ac)

SOLUTION

(mL/min)

(mL/min)

V0 (mL/min)

313
256
206
152
101
53

331
253
204
154
103
51

644
509
410
306
204
104

0.621
0.786
0.976
1.307
1.961
3.846

CONDUCTIVITY

CONVERSION,

(mS/cm)
1
2nd

st

inlet
7.2
7.1
6.9
6.5
6.1
5.3

outlet
6.6
5.8
5.6
5.1
4.8
4.2

(%)
101.8
103.0
102.6
103.2
106.2
108.2

REACTION
RATE
CONSTANT
(L/mol.min)
-910.54
-436.89
-404.48
-246.71
-87.36
-0.20

RATE OF
REACTION
(mol/L.min)
-2.95 x 10-3
-3.93 x 10-3
-2.73 x 10-3
-2.53 x 10-3
-3.36 x 10-3
-1.34 x 10-5

13

CONVERSION vs RESIDENCE TIME

110
108

f(x) = 1.97x + 101.05

106

Conversion, X (%)

104
102
100
98
0

0.5

1.5

2.5

3.5

4.5

Residence time, (min)

Experiment 3:
14

TITRATION SAMPLE

VOLUME of NaOH (mL)

AVERAGE VOLUME of

1st TRIAL

2nd TRIAL

300

25.00

25.90

25.45

250

25.50

26.00

25.75

200

25.90

25.40

25.65

150

25.90

26.00

25.80

100

26.10

27.00

26.55

50

25.70

26.60

27.05

(mL)

NaOH (mL)

SAMPLE CALCULATION

EXPERIMENT 2 and 3:

NaOH + HCl

NaCl + H2O

Unknown quantity
Concentration of NaOH in the reactor, CNaOH

= 0.1 M

Known quantities
Volume of sample, Vs

= 50 mL

Concentration of NaOH in the feed vessel, CNaOH,f

= 0.1 M

Volume of HCI for quenching, VHCI,s

= 10 mL

Concentration of HCI in standard solution, CHCI,s

= 0.25 M

Volume of titrated NaOH, V1

= 25.45 mL

Concentration of NaOH used for titration, CNaOH,s

= 0.1 M
15

Sample Calculation (for sample flow rate of 300ml/min)

Concentration of NaOH entering the reactor, CNaOH,o
= (CNaOH,f)/ 2
=

0.1
2

= 0.05 mol/L

Volume of unreacted quenching HCI, V2

=

C NaOH , s
C HCI , s

0.1
0.25

x V1

x 25.45

= 10.18 mL

Volume of HCI reacted with NaOH in sample, V3

= VHCI,s - V2
= 10 10.18
= - 0.18 mL

Moles of HCI reacted with NaOH in sample, n1

= CHCI,s x V3
= 0.25 x

0.18
1000

= -4.5 x 10-5 mol

Moles of unreacted NaOH in sample, n2 = n1

= -4.5 x 10-5 mol

16

Concentration of unreacted NaOH in the recator, CNaOH

= n2 / ( Vs / 1000 )
=

4.5 x 105
50
1000

= -9.0 x 10-4 mol/L

Conversion of NaOH in the reactor, X

= (1 -

C NaOH
C NaOH ,o

9.0 10
= (1
0.05

) x 100%

) x 100 %

= 101.8 %

Residence time,
=

V ( PFR )
Vo

0.4 L
644 mL/min

1000 mL
1L

= 0.621 min

Rate constant, k
=

Vo
V ( PFR ) CA 0

X
1X

where X is taking from the calculation in experiment 2

=

644 /1000
0.4 x 0.1

1.018
11.018

= -910.54 L/mol.min

17

Rate of reaction, -r
2
= k C A 0 (1-X)2

= (-910.54)(0.1)2(1-1.018)2
= -2.95 x 10-3 moL/L.min

DISCUSSION
There are three experiments for plug flow reactor (PFR). These experiments are
conducted to achieve a few objectives, which are to carry out a saponification reaction
between NaOH and Et(Ac) in a PFR, to determine the rate of reaction, the conversion of
NaOH in the reactor and to find the effect of residence time on the conversion in a plug
flow reactor (PFR).
18

In experiment one, the conductivity meter is used to measure the conductivity in

the two solutions which are sodium hydroxide, NaOH and sodium acetate, Na(Ac). Using
the same concentration but different volume of each solution is conducted to achieve
desire conversion. Then, the conductivity for each new solution that has being mixed is
tested by conductivity meter. The calibration curve of conductivity versus conversion is
plotted. The slope of this graph is -0.0782 and y-axis intercept is 12.472. The conductivity
lower when the conversion is increased.
For the next experiment, the plug flow reactor (Model:BP 101) is used. The feed of
sodium hydroxide, NaOH and ethyl acetate, Et(Ac) is varied to get different of residence
time, . The theory of residence time distributions generally begins with three
assumptions which are the reactor is at steady-state, transport at the inlet and the outlet
takes place only by advection, and the fluid is incompressible 4. For each different residence
time, the 50 mL of sample is collected and being back titrate with hydrochloric acid to
determine the concentration of sodium hydroxide, NaOH in that sample. Then, the
conversion of NaOH in the reactor is calculated. The graph of conversion of NaOH and
residence time is plotted. This graph shows that the conversion is increase as the residence
time increase. For the real case, the conversion must increase as the residence time
increase5. However, the conversion that is calculated is weird because the conversion is
higher than 100%. From the conversion value, the rate constant and rate of reaction can be
calculated too. All the rates of reaction that are get from the calculation are negative
values. These happened because the conversion values are more than 100%.
Therefore, it can say that there are errors occurs during conducted this experiment. One of
the errors that can happened in this experiment is there are impurities in the conical flask
during the titration process. This can affect the amount of sodium hydroxide solution
used. Next, maybe there was some leakage at any valve that did not noticed during
conduct the experiment. Other than that, the colour obtained during titration does not
4 Levenspiel, O., Chemical Reaction Engineering (3rd edition). John Wiley & Sons, USA (1999).

5 Research Saponification of Ethyl Acetate by Sodium Hydroxide in a Plug Flow Reactor by Lindsey Kato, Shawna Togioka,
Luke Sugie (February 2, 2005)

19

exactly in light pink. So, it might affect the value of NaOH use and affect the calculations.
Plug flow reactors are frequently used in the chemical due to the non-mixing
property of the reactors. Plug flow reactors are used for some of the following applications
such as large-scale reactions, fast reactions, homogenous or heterogeneous reactions,
continuous production, and high-temperature reactions6.

CONCLUSION
This experiment is not perfectly success; however, the objectives of this experiment were
achieved. From this experiment, the collected data are sufficient but there are some errors
that are happened during run the experiment. For experiment 1, the graph of conductivity
versus conversion of sodium hydroxide using conductivity meter is inversely proportional.
Then, for next experiment, it can be concluded that the conversion of sodium hydroxide is
increase as the residence time increase. The graph shows that the conversion versus
6 http://en.wikipedia.org/wiki/Plug_flow_reactor_model#Applications
20

residence time is directly proportional. The experiment is said to not be perfectly

successful because the value of conversion of sodium hydroxide is exceed 100%.

RECOMMENDATION
There are a few suggestions to get more precise result for this experiment:

Run more trial on the experiment to get precise value especially in back titration
Ensure there are no leakage at the valve on the equipment
Make sure all the colour of titration should be in same colour which is light pink.
Make sure all valve correctly set up and are in right position.

21

REFERENCES

Books:
1. H. Scott Fogler, Elements of Chemical Reaction Engineering, 4 th Edition, Pearson
International Edition (2006).
2. Levenspiel, O., Chemical Reaction Engineering (3rd edition). John Wiley & Sons, USA
(1999).
3. Smith J.M., Chemical Engineering Kinetics, Mc Graw Hill (Singapore), 1981.
4. Astarita G., Mass Transfer with Chemical Reaction, Elsevier, 1967.
22

Internet:
1. http://www.scribd.com/doc/29195386/Plug-Flow-Reactor
2. http://en.wikipedia.org/wiki/Plug_flow_reactor_model
3. http://en.wikipedia.org/wiki/Plug_flow_reactor_model#Applications

Others:
1. Plug Flow Reactor, Product Description by Matthew Grisewood
2. Research Saponification of Ethyl Acetate by Sodium Hydroxide in a Plug Flow
Reactor by Lindsey Kato, Shawna Togioka, Luke Sugie (February 2, 2005)

APPENDIX

23

Conductivity meter

Plug flow reactor (Model: BP 101)

24