ABSTRACT

From this experiment, our objectives are to carry out the saponification reaction between NaOH
and Et(Ac) in plug flow reactor, to determine the reaction rate constant and the rate of reaction of the
saponification process. A unit called SOLTEQ Plug Flow Reactor (Model: BP 101) is used in this
experiment, commonly known as PFR. During the reaction we used Sodium hydroxide (NaOH) and Ethyl
acetate Et(Ac) as the reactant .The value of reaction rate constant and rate of reaction were calculated
from the data recorded. The reaction rate constant for 600ml/min flow rate was 102.19L/mol.min, for
the 500mL/min reaction rate constant was 52.60L/mol.min, for the 400mL/min reaction rate constant
was 52.50L/mol.min, for the 300mL/min reaction rate constant was 29.26L/mol.min, for the 200mL/min
reaction rate constant was 28.78L/mol.min and for the 100mL/min reaction rate constant was
13.13L/mol.min. Other than that, the rate of reaction for this process also determined. The rate of
reaction we got for flow rate of 600ml/min was 0.0170mol/L.min, for the 500mL/min the rate of
reaction was 0.0190mol/L.min,for the 400mL/min the rate of reaction was 0.0130mol/L.min, for the
300mL/min the rate of reaction was 0.0120mol/L.min, for the 200mL/min the rate of reaction was
0.0063mol/L.min and for the 100mL/min the rate of reaction is 0.0034mol/L.min. . A graph of
conductivity against conversion was plotted. From the graph, the conversion is inversely proportional to
the conductivity. So that, as the conversion increases, the conductivity decreases. A graph of conversion
against residence time also plotted. From the graph we can see that, the conversion of reaction changes
constantly as the residence time increases.













INTRODUCTION
Reactors play an important role in many production facilities involving the chemical
transformation of substances. Their performance determines the reliability and suitability of a process,
its environmental safety, the consumption of energy and the raw materials required. Chemical reactors
are vessels that contain chemical reactions. Different types of chemical, biological and physical
processes take place in reactors. Some examples of reactors include lakes, rivers, and sedimentation
tanks. The degree of mixing and residence time in reactors affect the degree of completion of reactions
within the reactor. (Dipa Dey et.al , 2007).
A plug flow reactor (PFR) is a type of chemical reactor where the influent is pumped into the
pipe. Chemical reactions occur through the length of the PFR and the reaction rate is not a constant. It is
also a vessel through which flow is continuous, usually at steady state with conversion of the chemicals
and other dependent variables are functions of position within the reactor rather than of time. In the
ideal plug flow reactor, the fluids flow as if they were solid plugs or pistons, and reaction time is the
same for all flowing material at any given tube cross section. Flow in these reactors can be laminar, as
with viscous fluids in small-diameter tubes while turbulent, as with gases. Turbulent flow generally is
preferred to laminar flow, because mixing and heat transfer are improved. (Laboratory of Environmental
and Science Engineering, n.d). For slow reactions and especially in small laboratory and pilot-plant
reactors, establishing turbulent flow can result in inconveniently long reactors or may require
unacceptably high feed rates.

Figure 1: Plug flow reactor


It is difficult to classify industrial chemical apparatus due to their diversity; however, a distinction is
made between stirred tank reactors and plug flow reactors.
Stirred tank reactors are mainly characterized by the following features:
o Perfect mixing allows the reaction to take place in the entire reactor volume and avoids the
formation of stagnant zones.
o Inlet concentration is not equal to the outlet concentration.
o The particle residence time distribution is the arithmetic mean of the residence time of all
particles.
o The reactor can be operated under isothermal conditions at steady state. This condition allows
the reactor to be easily controlled.
o The process temperature can be varied in a cascade of stirred reactors from one reactor to
another. The stable mode of operation can be achieved when each reactor in the cascade is
under isothermal conditions.

The features of a plug flow continuous reactor are as follows:
Flow is laminar, the properties of the reaction medium (i.e. pressure, temperature, reactant and
product concentrations) are the same throughout the entire cross section of flow.
All the elemental volumes of the reaction medium remain in the reactor for the same period of
time, and the change in concentration, temperature, and pressure with time are identical for
each elemental volume.
Additionally, there are temperature and reactant concentration gradients along the length of
the reactor.
The rate of chemical reactions vary along the length of the reactor.

OBJECTIVE
To carry out a saponification reaction between NaOH and Et(Ac) in a TFR.
To determine the reaction rate constant.
To determine the effect of residence time on the conversion in a TFR

THEORY
The Plug Flow Reactor (PFR) is used to model the chemical transformation of compounds as they
are transported in pipes. The pipe may represent a river, a region between two mountain ranges
through which air flows, or a variety of other conduits through which liquids or gases flow. Besides, it
can even represent a pipe.(Richard E. Honrath, n.d).In an ideal tubular flow reactor, specific assumptions
are made regarding the extent of mixing:
No mixing in the axial direction
Complete mixing in the radial direction
A uniform velocity profile across the radius
Rate of reaction and rate law
Simply put, rate of reaction can be roughly defined as the rate of disappearance of
reactants or the rate of formation of products. When a chemical reaction is said to occur, a reactant(or
several) diminishes and a product(or several) produced. This is what constitutes a chemical reaction. For
example
aA + bB cC + dD (Equation 1.1)
Where A and B represent reactants while C and D represent products. In this reaction, A and B is
being diminished and C and D is being produced. Rate of reaction, concerns itself with how fast the
reactants diminish or how fast the product is formed. Rate of reaction of each species corresponds
respectively to their stoichiometric coefficient. As such :

(Equation 1.2)
Rate of equation for reactant A is:

(Equation 1.3)
k =rate constant

= concentration of A species

=concentration of B species
=stoichiometric coefficient of A
=stoichiometric coefficient of B
The rate expression can be shown to be
-r
A
= k [A] [B] (Equation 1.4)
Where if [A] is equal to [B], this simplify to
-r
A
= k [A]
2
(Equation 1.5)
In the general case the order of the reaction is not known and is shown by
-r
A
= k [A]

If the inlet concentration, [A] is known, k can be determined. The reaction:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
Sodium Hydroxide + Ethyl Acetate Sodium Acetate + Ethyl Alcohol
can be considered equal-molar and first order with respect to both sodium hydroxide and ethyl acetate
i.e. second order overall, within the limits of the concentration (0-0.1M) and temperature (20-40
o
C)
studied. (Instruction Manual Turbular Flow Reactor,2006)
Conversion
While conversion shows how many moles of products are formed for every mole of A has consumed.

(Equation 1.6)

Residence Time Distribution (RTD)
Residence Time Distribution is a characteristic of the mixing that occurs in the chemical reactor.
There is no axial mixing in a plug flow reactor, PFR and this omission can be seen in the Residence Time
Distribution, RTD which is exhibited by this class of reactors. The continuous stirred tank reactor CSTR is
thoroughly mixed and its RTD is hugely different as compared to the RTD of PFR.

APPARATUS
Plug Flow Reactor Model Bp101
Burette
Measuring cylinder
Beakers
pH indicator
Conical flask
0.1M Sodium Hydroxide, NaOH
0.1M Ethyl Acetate, Et(Ac)
0.1M Hydrochloric Acid, HCl
De-ionized water


Figure 2 : Plug flow reactor


PROCEDURE
General Start-up Procedures
1. All the valves are ensured closed except V4, V8 and V17.
2. The following solutions are prepared: 20 liter of NaOH (0.1M) 20 liter of Et(Ac) (0.1M)1 liter of
HCL (0.25M) for quenching
3. Feed tank B1 was filled with NaOH while feed tank B2 was filled with the Et(Ac).
4. The water jacket B4 was filled with water and pre-heater B5 was filled with clean water.
5. The power for the control panel was turned on.
6. Valves V2, V4, V6, V8, V9 and V11 were opened.
7. Both pumps P1 and P2 were switched on. P1 and P2 were adjusted to obtain flow rate
approximately 300mL/min at both flow meters Fl-01 and Fl-02. Both flow rates were made sure
to be equal.
8. Both solutions then were allowed to flow through the reactor R1 and overflow into waste tank
B3.
9. Valves V13 and V18 was opened. Pump P3 then was switched on in order to circulate the water
through pre-heater B5. The stirrer motor M1 was switched on and set up to speed about200
rpm to ensure homogeneous water jacket temperature.
Experiment Procedures
1) The general starts 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 metersFI-01
and FI-02. Both flow rates were ensured same. The flow rates were recorded.
5) The inlet (QI-01) and outlet (QI-02) were started to monitor the conductivity values 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.
7) Optional: Sampling was opened from valve V15 and 50ml of sample was collected. A
back titration procedure was carried out manually to determine the concentration of NaOH in
the reactor and extent of conversion.
8) The experiment was repeated from step 4 to 7 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 made sure to be equal.
Titration Procedures
1. The burette was filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl was poured in a flask.
3. 50 mL 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.













RESULT
Conversion Solution Mixtures Concentration
of NaOH (M)
Conductivity
(mS/cm)
0.1M NaOH 0.1M Na(Ac) Water
0% 100mL - 100mL 0.0500 6.31
25% 75mL 25mL 100mL 0.0375 5.25
50% 50mL 50mL 100mL 0.0250 4.55
75% 25mL 75mL 100mL 0.0125 3.71
100% - 100mL 100mL 0.0000 2.55
Table 1: Preparation of Calibration Curve
Reactor volume: 4L
Concentration of NaOH in feed tank: 0.1M
Concentration of Et(Ac) in feed tank: 0.1M
No Flow
rate of
NaOH
(mL/min)
Flow
rate of
Et(Ac)
(mL/min)
Total
flow rate
of
solutions,

(mL/min)
Residence
time,
(min)
Outlet
conductivity
(mS/cm)
Volume
of
NaOH
(ml)
Conversion,
X (%)
Reaction
Rate
Constant
(L/mol.min)
Rate of
Reaction
(mol/L.min)
Q1 Q2
1 300 300 600 0.667 7.7 6.9 0.0218 87.2 102.19 0.0170
2 250 250 500 0.800 7.2 6.2 0.0202 80.8 52.60 0.0190
3 200 200 400 1.000 6.8 5.7 0.0210 84.0 52.50 0.0130
4 150 150 300 1.333 6.7 5.5 0.0199 79.6 29.26 0.0120
5 100 100 200 2.000 6.4 5.2 0.0213 85.2 28.78 0.0063
6 50 50 100 4.000 5.8 4.5 0.021 84.0 13.13 0.0034
Table 2: Experiment 3




CALCULATION
Residence time

For flow rate of 300 mL/min
Total flow rate, V
0
= Flow rate of NaOH + Flow rate of Et(Ac)
= 300 mL/min NaOH + 300 mL/min Et(Ac)
= 600 mL/min = 0.6 L/min
Reactor volume, V = 0.4 L

Conversion
(

)

For flow rate of 300 mL/min
Volume of sample, V
s
= 50 mL = 0.050 L
Concentration of NaOH in the feed vessel, C
NaOH, f
= 0.1 mol/L
Volume of HCl quenching, V
HCl
= 10 mL = 0.010 L
Concentration of HCl in standard solution, C
HCl
= 0.25 mol/L
Volume of NaOH titrated, V
1
= 21.8 mL = 0.0218 L
Concentration of NaOH used for titration, C
NaOH, s
= 0.1 mol/L

)
(

)





Reaction rate constant, k

)
X = extent of conversion
v
0
= total flow rate of solution (L/min)
C
A0
= Inlet concentration of reactant NaOH in the reactor (mol/L)
V = Reactor volume (L)
For flow rate of 300 mL/min



(

Rate of reaction, -r
A

-r
A
= kC
2
A0
(1-X)
2
For flow rate of 300 mL/min

Figure 3: Conductivity (mS/cm) versus Conversion(%)



Figure 4: Conversion, X (%) versus Residence time, (min)


0
1
2
3
4
5
6
7
0% 20% 40% 60% 80% 100% 120% 140%
C
o
n
d
u
c
t
i
v
i
t
y

(
m
S
/
c
m
)

Conversion
Conductivity (mS/cm) vs. Conversion
79
80
81
82
83
84
85
86
87
88
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
C
o
n
v
e
r
s
i
o
n
,

X

(
%
)

Residence time, (min)
Conversion, X (%) vs. Residence time,(min)
DISCUSSION
The objective of this experiment to carry out a saponification reaction between NaOH and Et(Ac)
in a plug flow reactor. Besides, we determine the reaction rate constant and the effect of residence time
on the conversion in plug flow reaction. Saponification is a process that produces soap, usually from fats
and lye. The process involves a reaction between a base, usually sodium hydroxide (caustic soda), and
an ester group on a compound. For this experiment, we conducted saponification process in plug flow
reactor Model Bp101.So the reaction occurred different resulted. During the reaction we used Sodium
hydroxide (NaOH) and Ethyl acetate Et(Ac) as the reactant .
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Sodium Hydroxide + Ethyl Acetate Sodium Acetate + Ethyl Alcohol
By using a Plug Flow Reactor, PFR, these two substances were flowed into the reactor, mixed
and react for a certain period of time to completing the saponification process .Both the NaOH and
Et(Ac) solutions were allowed to enter the plug reactor and empty into the waste tank .P1 and P2 were
adjusted to give a constant flow rate of about 300 ml/min at flow meters FI-01 and FI-02. Both flow
rates were ensured same. The flow rates were recorded. The flow rate of reaction was set up from 300
ml/min to 50 ml/min for both NaOH and Et(Ac) flow rate. Sampling was opened from valve V15 and
50ml of sample was collected. A back titration procedure was carried out to determine the
concentration of NaOH in the reactor and extent of conversion. Titration was carried out between 0.1 M
of NaOH with 0.1M HCI and sample from reaction added 3 drops of phenolphthalein. The volume of
NaOH change the colour of solution to light pink was recorded.
After that, the conversion of the reaction and rate constant can be calculated. The reaction rate
constant for flow rate 600ml/min is 102.19 L/mol.min while flow rate 500 ml/min is 52.60 L/mol.min.
Next, for flow rate 400ml/min,300 ml/min and 200 ml/min the rate constant are 52.50
L/mol.min,29.26L/mol.min and 28.78 L/mol.min respectively. The reaction rate constant is 13.13
L/mol.min for flow rate 100 ml/min. From these results, we can see that as the flow rate increases, the
reaction rate also increases.
Conversion is a property that shows how much of the reaction has taken place.For the
conversion of reaction, at flow rate 600ml/min and 500 ml/min are 87.2% and 80.8 % respectively. For
flow rate 400ml/min the conversion reaction was 84%.Besides that, conversion reaction for flow rate
300ml/min ,200 ml/min and 100 ml/min are 79.6%,85.2% and 84% respectively.As a result, the
conversion of reaction depends on the volume of NaOH from titration. The increase volume of NaOH
from titration, the more conversion of reaction occurred.
The rate of reaction also can be determined after we had done find the reaction rate constant.
From the resulted, the rate of reaction for 600ml/min was 0.0170 mol/L.min and for 500ml/min was
0.0190 mol/L.min. Other than that, reaction rate for 400ml/min,300 ml/min and 200ml/min was 0.0130
mol/L.min,0.0120 mol/L.min and 0.0063 mol/L.min respectively. The reaction rate was 0.0034mol/L.min
for flow rate 100ml/min. Therefore, the rate of reaction increases as the flow rate increases. At 600
ml/min the reaction rate decrease from 0.019 mol/L.min to 0.017 mol/L.min. This is maybe due to the
same value of the flow rate and the volume of the tank reactor.
A graph of conductivity against conversion was plotted. From the graph, the conversion is
inversely proportional to the conductivity. So that, as the conversion increases, the conductivity
decreases. Furthermore, a graph of conversion against residence time also plotted. From the graph we
can see that, the conversion of reaction changes constantly as the residence time increases.Therefore,
residence time is not a factor of reaction conversion. This is because PFR lacks a good mixing process.
Since the PFR is designed not to stir the solution vigorously to maximise mixing process, the conversion
of the reaction by using PFR is fairly low.










CONCLUSION
As a conclusion, we had carried out a saponification reaction between NaOH and Et(Ac) in a plug
flow reactor. Besides ,we had determined the reaction rate constant and the effect of residence time
on the conversion in PFR. The reaction rate constant for flow rate 600ml/min is 102.19 L/mol.min while
flow rate 500 ml/min is 52.60 L/mol.min. Next, for flow rate 400ml/min,300 ml/min and 200 ml/min the
rate constant are 52.50 L/mol.min,29.26L/mol.min and 28.78 L/mol.min respectively. The reaction rate
constant is 13.13 L/mol.min for flow rate 100 ml/min. So that, the flow rate increases, the reaction rate
also increases. Other than that, we also determined the rate of reaction. From the resulted, the rate of
reaction for 600ml/min was 0.0170 mol/L.min and for 500ml/min was 0.0190 mol/L.min. Then, reaction
rate for 400ml/min,300 ml/min and 200ml/min was 0.0130 mol/L.min,0.0120 mol/L.min and 0.0063
mol/L.min respectively. The reaction rate was 0.0034mol/L.min for flow rate 100ml/min. Therefore, the
rate of reaction increases as the flow rate increases. At 600 ml/min the reaction rate decreases from
0.019 mol/L.min to 0.017 mol/L.min. This is maybe due to the same value of the flow rate and the
volume of the tank reactor. A graph of conductivity against conversion was plotted. From the graph, the
conversion is inversely proportional to the conductivity. So that, as the conversion increases, the
conductivity decreases. A graph of conversion against residence time also plotted. From the graph we
can see that, the conversion of reaction changes constantly as the residence time increases.Therefore,
residence time is not a factor of reaction conversion. The experiment is conducted and completed
successfully.











RECOMMENDATION
There are several recommendations that can be taken in order to get more accurate result that are:
1. Before carry out the experiment, please consult with technician on how to run the equipment so
that you can save your time and energy while doing the experiment.
2. It is recommended that this experiment should be repeated at various other temperatures to
investigate the relationship between the reaction rate constant and the rate of reaction.
3. It is further recommended that the experiment be repeated using dissimilar flow rates for the
NaOH solution and ethyl acetate solutions to investigate the effect that this will have upon the
saponification process.
4. For obtained more accurate results, run several trials on tubular flow reactor so we can take the
average value from each different molar rates.
5. Be careful when doing the titration because we only want the last drop of NaOH that will convert
the solution to light pale purple colour. The excess of drop of NaOH will give effect on the result
in the calculations.


REFERENCE
Laboratory of Environmental and Science Engineering. (n.d) .Bioreactors for metal bearing
wastewater treatment: Tubular Reactor or Plug flow reactor. Retrieved from:
http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm
Dipa Dey, Amanda, Herzog , Vidya Srinivasan.(2007).Tracer Studies In a Plug Flow Reactor.
Retrieved from:
http://www.egr.msu.edu/~hashsham/courses/ene806/docs/Plug%20Flow%20Reactor.pdf
Richard E. Honrath.(n.d).CPE521,Mass and energy balance . Retrieved from
:http://www.cee.mtu.edu/~reh/courses/ce251/251_notes_dir/node3.html
Instruction Manual Turbular Flow Reactor.(2006).Retrieved from
:http://eleceng.dit.ie/gavin/DT275/CET%20MKII%20manual%20issue%2016.pdf
Laboratory Manual Tubular Flow Reactor .Retrieved from:
http://www.solution.com.my/pdf/BP101(A4).pdf





APPENDIX