UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY III
(CHE574)
NAME

: EDZHARFARIZ BIN TAMIN

2013594311
: SHAHRIZAT BIN SMAIL KASSIM
2013197421
: KHATIJAH BINTI MOKHTAR
2013934197
: NURAMANINA BT MOHD SOHADI 2013520381
GROUP
: EH2204
EXPERIMENT
: 2. PLUG FLOW REACTOR
DATE PERFORMED : 30TH OCTOBER 2015
SEMESTER
:4
PROGRAMME / CODE : EH220
SUBMITTED TO
: MADAM FAZLIANI BINTI SHOPARWE
No.
1
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3
4
5
6
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11
12

Title
Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference / Appendix
TOTAL MARKS

Remarks:
Checked by :
--------------------------Date :

Allocated Marks (%)

5
5
5
5
5
10
10
10
20
10
5
10
100

Marks

TABLE OF CONTENTS

1.0

Abstract

2.0

Introduction

3.0

Objectives

4.0 Theory

5.0

Materials and Apparatus

6.0

Procedures

7.0

6.1 General Start-up Procedure

6.2 Experimental Procedure

6.3 Back Titration Procedure

6.3 General Shut-down Procedure

Results
7.1 Data

10

7.2 Graph

11

8.0 Calculations

12

9.0 Discussions

18

10.0 Conclusion

20

11.0 Recommendations

20

12.0 References

21

13.0 Appendices

22

1.0

ABSTRACT

EFFECT OF RESIDENCE TIME ON THE REACTION

This experiment is carried out based on a few objectives. A saponification reaction
between sodium hydroxide, NaOH and Ethyl acetate, Et (Ac) by using SOLTEQ Plug Flow
Reactor (Model: BP 101) is conducted to determine the effect of residence time on the
conversion and to evaluate the reaction rate constant. Two solutions, Sodium Hydroxide,
NaOH and Ethyl Acetate, Et(Ac) were reacted in Plug Flow Reactor and then the product was
analysed by the method of titration, which is some common laboratory apparatus are used.
Titration process is conducted to determine how well did the reaction go. The result shows
that the conversion of Sodium Hydroxide, NaOH is slightly changed as residence time
increase from 6.667 min until 13.333 min. As it at 20.000 min, the conversion increases from
91.4% to 95.0%. Therefore, one can be postulate that the reason for this phenomenon is that
the Plug Flow Reactor have a good mixing process. This experiment also aims to evaluate the
rate of reaction and reaction rate constant, hence both these properties have been determined
in the calculation section.

2.0

INTRODUCTION

2.1

Basic Purpose of Reactors

Reactors are designed due to some purposes, which are for Mixing of substrates by
contacting with catalyst, mass and heat transfer, control and containment or
protection from/of environment (Heinzle, 2009).
2.2

Quantitative Description of Ideal Reactors

There are various criteria in selecting the optimal reactor. The reactors are already
installed and process conditions have to be adjusted to fit into the available
equipment in fermentation plants and typical fine chemical. However, mainly feeding
strategies can be optimized as far as the reactor is concerned (Heinzle, 2009).
In addition, according E. Heinzle, continuous processes are installed for a
production of large-scale. Reactor choice is important in order to build a new plant or
in certain cases for replacing an existing one. It is useful to study ideal reactors first
to improve more understanding. The reactors including the batch reactor (BR), the
plug flow reactor (PFR) and the continuous stirred tank reactor (CSTR).
2.3

Steady-State Plug Flow Reactor (PFR)

In this experiment, the Plug Flow Reactor (Model: BP 101) is used as it has been properly
designed especially for students in conducting an experiment on chemical reaction in liquid
phase under isothermal and adiabatic condition. By using this unit, students are capable to
conduct the typical saponification reaction between Sodium Hydroxide, NaOH and Ethyl
Acetate, Et(Ac) among the others reaction.
The material balance for a component A in a steady-state (dC i/dt=0) plug flow
reactor element of volume dV as shown in Figure 1.0 is
Equation 1.0

Figure 1.0: Plug Flow Reactor

3.0

OBJECTIVES

This experiment is conducted to carry out a saponification reaction between sodium

hydroxide, NaOH and Ethyl acetate, Et (Ac) by using SOLTEQ Plug Flow Reactor (Model:
BP 101) to determine the reaction rate constant. In addition, it is also to determine the effect
of residence time on the conversion.
To conducting this experiment, residence times have to be manipulated throughout the
experiment and the effects of each one is studied. Residence time is varied by the means of
changing the flow rates of the feed solutions. It can be seen that residence time is a function
of total flow rates of the feed.
Hence, several residence times can be obtained and the effect of each one is studied
by varying the flow rate of the feed solutions.
4.0

THEORY

4.1

Rate of reaction and Rate law

The rate of reaction can be defined as the change in the concentration of any one of reactants
or product per unit time. Normally, a reactant will diminish while a product will produce
when a chemical reaction is occurring.
The rate of reaction changes as the reaction under progress. Initially, the rate of
reaction is relatively large. However, the rate of reaction decreases to zero as the time flows.
At this point, the reaction is complete (Blauch, 2014).
Guldberg and Waage derived an equilibrium constant by defining equilibrium as the
condition when the rates of the forward and reserve reactions are equal. Consider constitutes
a chemical reaction as (Christian, 2004):
aA + bB

cD + dD

Equation 2.0

From equation above, A and B represent as the reactants, where is being dimished.
While C and D represent as the products which are being produced. Rate of reaction of each
species corresponds respectively to their stoichiometric coefficient as below:
Equation 3.0
The negative sign indicates the reactants. The products are always positives sign.
While a, b, c, and d is the number of moles for each species A, B, C, and D. Usually, equation
for rA is defined as:

Equation 4.0

Where,
k

: rate constant

CA

: concentration of A species

CB

: concentration of B species
: stoichiometric coefficient of A
: stoichiometric coefficient of B

The relationship between the concentration of reactant and the rate of reaction is
expressed by a rate law. The differential rate law describes how the rate of reaction varies
with the concentrations of various species, usually reactants, in the system (Blauch, 2014).
A rate law is a mathematical equation which describes the progress of the reaction that
must be determined experimentally. There are two types of a rate law for chemical kinetics,
which are differential rate law and the integrated rate law (Blauch, 2014).
Table 1.0 below shows the example of a species in the chemical reaction with the
corresponded reaction order, differential rate law and integrated rate law.
Table 1.0: Reaction order with differential and integrated rate law
Reaction Order
Zero

Differential Rate Law

Integrated Rate Law

First
Second

4.2

Conversion

Taking species A as the basis, the reaction expression can be divided through the
stoichiometric coefficient of species, hence the reaction expression can arranged as follows:
Equation 5.0

Conversion is an improved way of quantifying exactly how far has the reaction moved, or
how many moles of products are formed for every mole of A has consumed. Conversion XA is
the number of moles of A that have reacted per mole of A to the system as below:
Equation 6.0

4.3

Plug Flow Reactors

Reaction rate constant,

Equation 7.0

Where,
Vo

: Total inlet flow rate

VT

: Reactor Volume

CAo

: Inlet NaOH concentration

: Conversion

4.4

Residence Time Distribution Function

Plot a graph of conversion versus residence time. The reactors residence time is defined as
the reactor volume divided by the total feed flow rates.
Residence time,
Equation 8.0

5.0

MATERIALS/APPARATUS

The unit used for this experiment in SOLTEQ Plug Flow Reactor (Model: BP 101). It is used
as it has been properly designed for students experiment on chemical reactions in liquid
phase under isothermal and adiabatic conditions.
The chemicals used are 0.1M Sodium Hydroxide, NaOH, 0.1M Ethyl Acetate, Et
(Ac), 0.1M Hydrochloric Acid, HCl, and deionized water. Apart from that, there were also
some laboratory apparatus involved such as burette, conical flask, measuring cylinder, pH
indicator, and beakers.
The unit of jacketed plug reactor is also included, which is the individual reactant feed
tanks and pumps, temperature sensors and conductivity measuring sensor. Figure 2.0 shows
the unit SOLTEQ Plug Flow Reactor (Model: BP 101).

Figure 2.0: SOLTEQ Plug Flow Reactor (Model: BP 101)

6.0

PROCEDURES

6.1

General start-up procedure

1. All valves are ensured that initially closed except valves V4, V8 and V17.

2. The solutions are prepared for each experiment:

Table 2.0: Tanks B1 and B2
Tank

Experiments 1&2

Experiment 3&4

B1

Deionized water

0.1M NaOH solution

B2

0.05M NaCl solution

0.1M Et(Ac) solution

The water deionized is connected to the laboratory water supply.

3. The power for control panel is turned on.
4. The water jacket B4 and pre heater B5 are filled with clean water. Valves V13 and V18 are
opened. Pump P3 is switched on to circulate the water through pre heater B5.
5. The stirrer motor M1 is switched on and the speed is set up to about 200rpm.
6. Valves V2, V4 and V10 are opened. Pump P1 is switched on. P1 is adjusted to flow rate of
150 ml/min at flow meter FI-01. Valves V10 is closed and pump P1 is switched off.
7. Valves V6, V8 and V12 are opened. Pump P2 is switched on. P2 is adjusted to flow rate of
150 ml/min at flow meter FI-02. Valve V12 is closed and pump P2 is switched off.
8. The unit is now ready for the experiment.

6.2

Experimental procedure
1. The general start-up procedure was 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 F101 and F1-02. Both flow rates were make sure to be the same. The flow rates were recorded.
5. The inlet (QI-01) and outlet (QI-02) conductivity values were start 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
determined.
7. Optional: Sampling valve V15 was opened and 50 ml sample was collected. Titration
procedure was carried out to manually determine the concentration NaOH in the reactor and
extent of conversion.
8. Steps 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. Both flow rates were make
sure to be the same.

6.3

Back Titration Procedure

1. The burette was filled up with 0.1M NaOH solution.
2. 10mL of 0.25M HCl was poured in a flask.

3. 50mL samples that were collected from the experiment at every controlled flow rate (300,
250, 200, 150, 100 and 50 ml/min) were added into the 10ml HCl to quench the
saponification reaction.
4. 3 drops of phenolphthalein were dropped into the mixture of sample and HCl.
5. The mixture then was titrated with NaOH until it turns light pink.
6. The amount of NaOH titrated was recorded.

6.4

General shut-down procedure

1. Pumps P1, P2 and P3 are switched off. Valves V2 and V5 are closed.
2. The heaters are switched off.
3. The cooling water is kept circulated through the reactor while the stirrer motor is running to
allow the water jacket to cool down to room temperature.
4. If the equipment is not going to be used for long period of time, all the liquid is drained from
the unit by opening valves V1 to V19. The feed tanks are rinse with clean water.
5. The power is turned off for the control panel.

7.0

RESULTS

Table 7.1: Table for preparation of calibration curve.

Conversion
(%)
0
25
50
75
100

0.1 M

Solution mixtures (mL)

0.1 M

NaOH
100
75
50
25
-

Na(Ac)
25
50
75
100

100
100
100
100
100

Concentration

Conductivity

of NaOH (M)

(mS/cm)

0.0500
0.0375
0.0250
0.0125
0.0000

17.05
14.55
11.45
9.82
7.96

Graph 7.1: Graph of conductivity versus conversion.

Table 7.2: Effect of residence time on the reaction.

Reactor volume

=4L

Concentration of NaOH in feed tank = 0.1 M

Concentration of Et(Ac) in feed tank = 0.1 M
No

Flow rate

Flow rate

Total flow

of NaOH

of Et(Ac)

rate of

(mL/min) (mL/min)

1
2
3
4

300
250
200
150

300
250
200
150

solution,
(mL/min)
600
500
400
300

Residence
time,
(min)
6.6667
8.0000
10.0000
13.3333

Outlet

Conversion

Reaction

Rate of

conductivity

X (%)

rate

reaction

constant (L

(mol/L.min)

(mS/cm)

/mol.min)
11.0
9.5
8.4
7.5

9.7
8.4
7.4
6.4

50.6
50.4
50.2
50.2

1.5364
1.2702
1.0080
0.7560

0.003749
0.003125
0.002499
0.001875

5
6

100
50

100
50

200
100

20.0000
40.0000

6.7
5.7

5.5
4.7

50.4
50.4

0.5081
0.2540

Table 7.3
Flow rate of NaOH
(mL/min)

Flow rate of Et(Ac)

(mL/min)

Residence time

300
250
200
150
100
50

300
250
200
150
100
50

5
5
5
5
5
5

Volume of NaOH,
(mL)
0.3
0.2
0.1
0.1
0.2
0.2

Graph 7.2: Graph of conversion versus residence time.

8.0

CALCULATIONS

Back titration for manual conversion determination:

Unknown quantity:
Concentration of NaOH in the reactor

mol/L = 0.1 mol/L

0.001250
0.000625

Known quantities:
Volume of sample

mL

Concentration of NaOH in the feed vessel

mol/L = 0.1 mol/L

Volume of HCl for quenching

mL

= 50 mL

= 10 mL

Concentration of HCl in standard solution

mol/L = 0.25 mol/L

Volume of titrated NaOH

mL

Concentration of NaOH used for titration

mol/L = 0.1 M

Sample calculations:
For flow rate = 300 mL/min

Concentration of NaOH entering the reactor,

Volume of unreacted quenching HCl,

Volume of HCl reacted with NaOH in sample,

Moles of HCl reacted with NaOH in sample,

Moles of unreacted NaOH in sample,

Concentration of unreacted NaOH in the reactor,

Conversion of NaOH in the reactor, X

For flow rate = 250 mL/min

Concentration of NaOH entering the reactor,

Volume of unreacted quenching HCl,

Volume of HCl reacted with NaOH in sample,

Moles of HCl reacted with NaOH in sample,

Moles of unreacted NaOH in sample,

Concentration of unreacted NaOH in the reactor,

Conversion of NaOH in the reactor, X

For flow rate = 200 mL/min

Concentration of NaOH entering the reactor,

Volume of unreacted quenching HCl,

Volume of HCl reacted with NaOH in sample,

Moles of HCl reacted with NaOH in sample,

Moles of unreacted NaOH in sample,

Concentration of unreacted NaOH in the reactor,

Conversion of NaOH in the reactor, X

Sample calculations of Residence Time, (min)

where

For flow rate = 300 ml/min

=
=

= 0.6 L/min

6.6667 min

For flow rate = 250 ml/min

= 0.5 L/min

8.0000 min

Other residence time were calculated by the same way, and varying the flow rates
Sample calculations of Reaction Rate Constant and Rate of Reaction

Flow rate = 300 mL/min

Flow rate = 250 mL/min

9.0

DISCUSSION

The experiment was conducted using plug flow reactor by SOLTEQ (model BP 101).
Plug flow reactor (PFR) is a type of reactor that consists of a cylindrical pipe and usually
operated at steady state. The feed enters at one end of a cylindrical tube and the product
leaves at the other end. The reactor has long tube and lack of provision for stirring, thus
preventing the fluid from mixing completely. So, the properties of the fluid will vary from
one and another. The solution in the tube is treated as a series of layers of volume segments
that are unmixed with the segment before and after it like a series of plugs that is stacked
together in a pipe. The plug flow reactor experiment was carried out to achieve several
objectives that is to carry out a saponification reaction between NaOH and Et(Ac), determine
the reaction rate constant and determine the effect of residence time on the conversion.
All the data needed were tabulated as seen in Table 7.1, 7.2 and 7.3. The first table
which is the preparation of calibration curve shows the conductivity of solution mixtures for
each percent conversion and varies concentration of NaOH. The conductivity values were
taken by using conductivity meters device. A graph of conductivity versus conversion is
plotted based on the results. From the graph, we can clearly see that as the percent conversion
increase from 0% to 100%, the conductivity kept on decreased. At 0% conversion with
0.0500 M of NaOH concentration, the conductivity reading shows value of 17.05 mS/cm. At
25% (0.0375 M NaOH), 50% (0.0250 M NaOH), 75% (0.0125 M NaOH) and 100% (0.0000
M NaOH) conversions, the conductivity values read as 14.55, 11.45, 9.82 and 7.96 mS/cm
respectively.
Next, we will discuss on the effect of residence time on the reaction and the results are
shown as seen in table 7.2 and 7.3. The volume of reactor used in this experiment is 4 L with
the concentration of 0.1 M for both NaOH and Et(Ac) in feed tank. The table 7.2 consist of
flow rate for both NaOH and Et(Ac), total flow rate of solutions, , residence time, ,outlet
conductivity, conversion, X, reaction rate constant,k and rate of reaction,

. For table 7.3, it

consists of residence time and the volume of NaOH titrated. These tables necessary to fill in
the results after the calculations were done.

The residence time was calculated by using the formula

where

. Total flow rate of solutions,

differ for each flow rates starting from 300

mL/min to 50 mL/min. From the calculations, the residence times in minutes calculated to be
6.6667, 8.0000, 10.0000, 13.3333, 20.0000 and 40.0000 for flow rates 300, 250, 200, 150,
100 and 50 mL/min respectively. For the calculation of the conversion,X in percent, there are
many steps to be done first before we get to conversion,X and it is all can be seen in

calculations sections. The formula to calculate the conversion is

. At

300 mL/min flow rate, the conversion is 50.6%, at 250, 100 and 50 mL/min flow rate, the
conversion is 50.4%. At flow rates of 200 and 150 mL/min shows the least percent
conversion of X with only 50.2%. So, with all these, we were able to plot a graph of
conversion versus residence time. Our objective which is to determine the effect of residence
time on the conversion is achieved.
Next, we proceed to determine the reaction rate constant as it is one of our main
objectives. The reaction rate constant can be determined by the formula;

As soon as we get the reaction rate constant,k ,we were able to calculate the rate of reaction.
The formula for rate of reaction is;
From the results, the reaction rate constant,k is the highest at 300 mL/min with 1.5364
and the trend decreases for each flow rates recorded. Flow rate of 50 mL/min
has the least value of reaction rate constant with 0.2540

. The same scenario can

be seen for rate of reaction where at 300 mL/min, the value recorded is 0.003749
and the lowest is 0.000625

for flow rate 50 mL/min.

In running the experiment, there may be errors occurred. We cannot afford to avoid
mistakes but analysis of errors for further improvement prior to the experiment can be done.
During taking the conductivity values, make sure the conductivity meter were rinsed with

distilled water every time we take the reading for every flow rates. If we do not do these, it
may affect the reading of the conductivity hence the overall success of the experiment.

10.0

CONCLUSION

This experiment is conducted to with several objectives. The first one is to carry out a
saponification process between Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac) by
using SOLTEQ Plug Flow Reactor (Model: BP 101). These two substances were let to flow
into the reactor from feed tank 1 and feed tank 2. Then, it is mixed and let to react for certain
period of time. Saponification process then was completed after it had done.
Furthermore, next objective is to study the residence of time with the conversion of
the reaction. The relationship was successfully studied and graphed in Figure 3.0. The
conversion of the reaction remains fairly constant and the changes are too small at the
residence time of 6.667 min until 13.333 min. As it at 20.000 min, the conversion increases
from 91.4% to 95.0%. it can be concluded that the Plug Flow Reactor has good mixing
process.
Lastly, this experiment is conducted to determine the reaction rate constant and rate of
reaction. This has been done by calculating the reaction rate as in calculation section. It
shows that those values decreasing as the residence time increasing.

11.0

RECOMMENDATIONS

There are some recommendations should be considered while conducting the SOLTEQ Plug
Flow Reactor (Model: BP 101). Pumps should never be run in dry and titration should be
immediately stopped when the indicator turned pink.
In addition, Flow rates should be constantly monitored so that it remains constant
throughout the reaction as needed. Next, all valves should be properly placed before the
experiment started and it is better to time the sample so well so that the time wasting in taking
samples can be reduced or, if possible, avoided.

12.0

REFERENCES
Ashe, R. From Batch to Continuous Processing. Chemical Engineering. October
2012, pp. 34-40. Print.

Blauch, D.N., (2014). Chemical Kinetics. Retrieved April 28, 2015 from
http://www.chm.david
o Son.edu/vce/kinetics/differentialratelaws.html

Catalano, S., Wozniak, A., Kaplan, K., Plegue, T. Plug Flow Reactor. Encyclopedia of
Chemical

Engineering

Equipment.

Retrieved

April

3,

2015

from

mich.edu/Pages/Reactors/PFR/PFR.html.

Christian, G.D., (2004). Rate Law. Analytical Chemistry, 6th ed., John wiley & Sons,
Inc., 111 River Street, Hoboken, pp.499-505.

Fogler, H.S. Elements of Chemical Reaction Engineering, 4th ed. Levenspeil. PrenticeHall, 2014. Print.

Heinzle, E., (2009). Introduction to Ideal Reactors. Technische chemie I, WS2009,

Chemical Reactors, pp. 1-18.

Siti Wahidah, (n.d.). Design of Ideal Reactor for Single Reaction. Chemical Reaction
Engineering, UiTM Shah Alam.

13.0

APPENDICES

Figure 6.0: Feed Tank, B1

Figure 7.0: Feed Tank, B2

Figure 8.0: Pre-heater, B5

Figure 9.0: Plug Reactor, R1

Figure 10.0: Control Panel

Figure 11.0: Pumps P1 and P2