No.

Title

Page

1.

Abstract

2.

Introduction

3.

Aims

4.

Theory

5.

Apparatus

6.

Procedure

10

7.

Results

11

8.

Calculations

17

9.

Discussions

19

10.

Conclusions

20

11.

Recommendations

21

12.

Reference

21

13.

Appendix

22

1.0 ABSTRACT
This experiment was conducted to to examine the effect of a pulse input and
step change in a tubular reactor and also to construct the residence time distribution
(RTD) function for tubular flow reactor by using SOLTEQ Tubular Flow Reactor
model: BP 101. It is a batch reactor, usually at steady state and flows continuously.
The reaction was flow at constant flow rate 700mL/min in experiment 1 and let it for
one minute before reading is taken every 30 seconds until the conductivity reading is
0.0.The results from graph 1 shows the highest conductivity is 2 mS/cm at minutes
0.5 and suddenly steeply decrease from 1.9 mS/cm to 0.1 mS/cm at minutes 1 to 2.5.
In experiment 2, the conductivity were observe every 30 seconds until the reading at
Q2 become constant at least three times. From graph 3, the outlet conductivity
increase sharply before it kept constant at 3 to 5 minutes. From both graph 1 and 3, it
can be seen the differences between both graph where graph 3 is in increase
smoothly while graph 1 decrease into a constant value.

2.0 INTRODUCTIONS
A tubular reactor is a vessel where its flows is continuous, usually at steady
state, and configured so that conversion of the chemicals and others dependent
variables are functions of position within the reactor rather of time. It is a kind of
batch reactor which can provide high driving forces initially which then diminish as
the reaction flow in the tubes. Fluids flow in this reactor can be laminar flow, in tubes
with small diameter as with viscous fluids, and it is greatly deviate from ideal plug
flow behaviour or turbulent flow as with gases.
Turbulent flow is generally preferred to laminar flow as to improve the mixing
and heat transfer process. Establising turbulant flow can occur in conveniently long
reactors or may need unacceptable high feed rates for slow reactions such as in
laboratory or in the pilot plant reactors. Sometimes, tubular reactors operates
adiabatically or with heat transfer through the wall. The temperature naturally will
rises along the direction of flow in exothermic reaction and falls if it is endothermic.
Excessive heat along the reaction progress need to be removed from the reaction
through the wall in order to prevent undesirable side reaction.
There are some applications of tubular flow reactors which are:

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions
High temperature reactions of Residence Time Distribution (RTD) analysis is a

very efficient diagnosis tool that can beused to inspect the malfunction of chemical
reactors. It is also useful in the estimation of effluent properties and modelling reactor
behaviour. Residence time distributions can be measured by introducing a nonreactive tracer into the system at the inlet. According to a known function, the change
of concentration of the tracer occur and response is found by measuring the
concentration of the tracer at the outlet. The physical characteristics of the fluid
3

should not be modify by the selected tracer, so do as hydrodynamic conditions, it

should not be modify by introduction of the tracer. Generally, the change in tracer
concentration will either be a pulse or a step.
The residence time distribution of a real reactor is deviated from that of an
ideal reactor, depending on the hydrodynamics within the vessel. Some dispersion
along the path of the fluid, which may be attributed to turbulence, a non-uniform
velocity profile or diffusion were indicates by a non-zero variance. If the mean of the
E(t) curve arrives earlier than an expected time,

it indicates that there is a

stagnant fluid within the vessel. If the residence time distribution curve shows more
than 1 main peak, it may indicates chanelling, parallel path to the exit, or strong
internal circulation.

3.0 OBJECTIVES
1) To examine the effect of a pulse input and step change input in a tubular flow
reactor.
2) To construct a residence time distribution (RTD) function for the tubular flow
reactor.
3) To determine the conductivity of the solution and the conversion of reactant
based on calibration curves.

4.0 THEORY
A tubular reactor is a vessel through which flow is continuous, usually
at steady state, and configured so that conversion of the chemicals and other
dependent variables are functions of position within the reactor rather than of time. In
the ideal tubular 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.
Tubular reactors resemble batch reactors in providing initially high driving forces,
which diminish as the reactions progress down the tubes. Tubular reactor are often
used when continuous operation is required but without back-mixing of products and
reactants.
Flow in tubular reactors can be laminar, as with viscous fluids in smalldiameter tubes, and greatly deviate from ideal plug-flow behavior, or turbulent, as
with gases. Turbulent flow generally is preferred to laminar flow, because mixing and
heat transfer are improved. 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.
Tubular reactor is specially designed to allow detailed study of important
process. The tubular reactor is one of three reactor types which are interchangeable
on the reactor service unit. the reactions are monitored by conductivity probe as the
conductivity of the solution changes with conversion of the reactant to product. This
means that the inaccurate and inconvenient process of titration, which was formally
used to monitor the reaction progress, is no longer necessary.
The residence-time of an element of fluid leaving a reactor is the length of time
spent by that element within the reactor. For a tubular reactor, under plug-flow
conditions, the residence-time is the same for all elements of the effluent fluid. (K. G.
Denbigh)
The procedure would be to carried out experiments with tubular reactor at
varying feed rates, measuring the extent of reaction of the stream leaving the reactor.
One possible method might to add inert gas to the acetaldehyde vapour in such
quantity that the change in density between entry and exit of the reactor could be
6

neglected. In that case, the batch reactor time and the residence-time would both be
equal to the space-time.
Using the result of experiment, apply equation below to determine n and k (
wil bw known from the stoichiometry).

Mf = various values of feed rate

= space-time
From experiment, it should be able to draw a curve of against xout, the slope of
which according to the first equation, should be

Taking the logarithm of both sides of equation, we can obtain

So, n and k can be obtain from the intercept and slope of the appropriate loglog plot. This approach that the experiments be isothermal (k and T outside the
integral in the first equation). If the reactor is not isothermal, then the first equation
must be written as

Where Tin is the temperature of the feed into the reactor

Therefore, when the effect of wall heat transfer and of velocity gradient
operate simultaneously they might, under rather special circumstance, give rise to a
more complex kind of temperature profile. However, the most commonly observed
profiles obtained with exothermic reactions in externally cooled reactors. The reason
why the elementary design method is erroneous when the transverse gradients are
appreciable arises from the extreme sensitivity of reaction rate to changes of
temperature.

5.0 APPARATUS AND MATERIALS

1) SOLTEQ Tubular Flow Reactor model: BP 101
2) Stop watch
3) 0.1 M sodium hydroxide
4) 0.1 M sodium acetate
5) Deionised water

Figure 1: SOLTEQ Tubular Flow Reactor

6.0 PROCEDURE
6.1 PREPARATION OF CALIBRATION CURVE
1 liter of sodium hydroxide,NaOH (0.1M), 1 liter of sodium acetate, Na(Ac)
(0.1M) and 1 liter of deionised water,H 2O solutions were prepared. The conductivity
and NaOH concentration for each conversions values were determined by mixing the
following solutions into 100 ml of deionised water:
a) 0% conversion: 100mL NaOH
b )25% conversion: 75mL NaOH + 25mL Na(Ac)
c) 50% conversion: 50mL NaOH + 50mL Na(Ac)
d) 75% conversion: 25mL NaOH + 75mL Na(Ac)
e )100% conversion: 100mL Na(Ac)
All data were recorded in the table of Appendix A.

6.2 EXPERIMENT 1: PULSE INPUT IN A TUBULAR FLOW REACTOR

The general start-up procedure was performed. Valve V9 was opened and
pump P9 was switch on. Pump P1 flow controller was adjusted to give a constant
flow rate of deionised water into the reactor R1 at approximately 700ml/min at FI-01.
Deionise water was let to continue flowing through the reactor until the inlet (QI-01)
and outlet (QI-02) conductivity values are stable at low levels. Both conductivity
values were recorded. Valve V9 was closed and pump P1 was switch off. Then, valve
V11 was opened and pump P2 was switch on. The timer was start simultaneously.
Pump P2 flow controller was adjusted to give a constant flow rate of salt solution into
the reactor R1 at700ml/min at FI-02. The salt solution was let to flow for 1 min before
it was reset and the timer was restart. This will start the time at the average pulse
input. Valve V11 was closed and pump P2 was switch off. Valve V9 was opened
quickly and pump P1 was switch on. The deionised water flow rate was always
ensure to maintained at 700m/min by adjusting P1 flow controller. Both inlet (QI-01)
and outlet (QI-02) conductivity values were start recorded at regular intervals of 30
10

seconds. The conductivity values were recorded continually until all readings were
almost constant and approach the stable low level values.

6.3 EXPERIMENT 2: STEP CHANGE INPUT IN A TUBULAR FLOW REACTOR

The general start-up procedures were performed. Valve V9 was opened and
pump P1 was switch on. Pump P1 flow controller was adjusted to give a constant
flow rate of deionised water into the reactor R1 at approximately 700ml/min at FI-01.
The deionised water was let to continue flowing through the reactor until the inlet (QI01) and outlet (QI-02) conductivity values were stable at low levels. Both conductivity
values were recorded. Valve V9 was closed and pump P1 was switch off. Then, valve
V11 was opened and pump P2 was switch on. The timer was start simultaneously.
Both the inet (QI-01) and outlet (QI-02) conductivity values were recorded at regular
intervals of 30 seconds. The conductivity values were continually recorded untill all
readings are almost constant.

11

7.0 RESULTS
7.1 EXPERIMENT 1: PULSE INPUT IN TUBULAR FLOW REACTOR
Flow rate = 700 mL/min
Input type = Pulse Input
Time

Conductivity (mS/cm)

(min)

Inlet

Outlet

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

0.3
0.2
0.2
0.2
0.2
0.2
0.1
0.2
0.2
0.2
0.2

1.9
2.0
1.9
0.9
0.3
0.1
0.1
0.0
0.0
0.0
0.0

Graph Conductivity against Time

2.5

1.5
Conductivity (mS/ cm)
1

0.5

0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
Time (min)

12

Graph 1: Outlet Conductivity against Time

Graph E(t) against Time

0.7
0.6
0.5
0.4
E (t)

0.3
0.2
0.1
0
0

0.5

1.5

2.5

3.5

4.5

5.5

Time (min)

Graph 2: E(t) against Time

Time

Outlet Conductivity

(min)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

(mS/min)
1.9
2.0
1.9
0.9
0.3
0.1
0.1
0.0
0.0
0.0
0.0

E(t)

t E(t)

0.608
0.640
0.608
0.288
0.096
0.032
0.032
0.000
0.000
0.000
0.000
2.304

0.000
0.320
0.608
0.432
0.192
0.080
0.096
0.000
0.000
0.000
0.000
1.728

(t-tm)2 E(t) dt
15.200
12.960
9.728
3.528
0.864
0.200
0.128
0.000
0.000
0.000
0.000
42.608

(t-tm)3 E(t) dt
-76.000
-58.320
-38.912
-12.348
-2.592
-0.500
-0.256
0.0000
0.0000
0.0000
0.0000
150.016

Mean residence time, tm =

t E ( t ) dt=1.1728
0

13

Second moment,

2= ( tt m )2 E ( t ) dt=42.608
0

Third moment, skewness,

s=

(ttm )3

3
2

1
3

= (6.5275) 2

E(t) dt

-150.016) = -8.9953

7.2 EXPERIMENT 2: STEP CHANGE INPUT IN A TUBULAR FLOW REACTOR

Flow rate = 700 mL/min
Input type = Step change
Time
(min)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

Conductivity (mS/cm)
Inlet

Outlet

2.5
2.5
2.6
2.5
2.6
2.6
2.6
2.6
2.6
2.6
2.6

0.0
1.2
2.3
2.6
2.7
2.8
2.8
2.8
2.8
2.8
2.8

14

Conductivity value against time

12
10
8
Conductivity (mS/ cm)

Y-Values

4
2
0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5
Time (min)

Graph 3: Outlet Conducivity against time

Time

Conductivity

C(t)

E(t)

tm

S3

(min)

Inlet

Cit

(Cit) /

tE(t) /

(t-tm)2E(t) /

(t-tm)3E(t) /

Cit

Cit

Cit

0.000
5.530x10-5
4.240x10-4
1.077x10-3
1.989x10-3
3.223x10-3
4.641x10-3
6.317x10-3
8.251x10-3
1.044x10-2
1.289x10-2
=4.931x10-2

0.000
2.650x10-5
4.060x10-4
1.549x10-3
3.812x10-3
7.717x10-3
1.333x10-2
2.115x10-2
3.156x10-2
4.491x10-2
6.157x10-2
=0.186

0.000
1.330x10-5
4.060x10-4
2.323x10-3
7.616x10-3
1.927x10-2
3.992x10-2
7.390x10-2
0.126
0.202
0.307
=0.778

Outlet

Cit
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

2.500
2.500
2.600
2.500
2.600
2.600
2.600
2.600
2.600
2.600
2.600

0.000
1.200
2.300
2.600
2.700
2.800
2.800
2.800
2.800
2.800
2.800

0.000
0.000
0.600
0.008
2.300
0.031
3.900
0.052
5.400
0.072
7.000
0.093
8.400
0.112
9.800
0.130
11.200
0.149
12.600
0.168
14.000
0.186
=75.200 =1.000

15

E (t) against Time

E (t)

0.2
0.18
0.16
0.14
0.12
0.1
0.08
0.06
0.04
0.02
0
0

Time (min)

Graph 4: E (t) against Time

16

8.0 SAMPLE CALCULATION

8.1 EXPERIMENT 1: PULSE INPUT IN A TUBULAR FLOW REACTOR

C ( t ) dt
0

Area = (

t1

= Area under the graph

t2

f ( t 1 ) + f (t 2)
2

For time (0-0.5)

: A=0.5(1.9+2)/2 = 0.975 g.min/m3

For time (0.5-1)

: A=0.5(2+1.9)/2 = 0.975 g.min/ m3

For time (1-1.5)

: A=0.5(1.9+0.9)/2 = 0.7 g.min/ m3

For time (1.5-2)

: A=0.5(0.9+0.3)/2 = 0.3 g.min/ m3

For time (2-2.5)

: A=0.5(0.3+0.1)/2 = 0.1 g.min/ m3

For time (2.5-3)

: A=0.5(0.1+0.1)/2 = 0.05 g.min/ m3

For time (3-3.5)

: A=0.5(0.1+0)/2 = 0.025 g.min/ m3

5

So the total area or

C ( t ) dt
0

= ( 0.975+0.975+0.7+0.3+0.1+0.05+0.025) = 3.125

g.min/m3
E (t)=

C (t)

C ( t ) dt
0

For example, at t=0, C(t)=1.9

E (t)=

1.9
=0.608
3.125

E ( t ) dt=total area under graph

0

17

Area, A =

(t 2t 1 )( E

t 2t 1
)
2

For (0-0.5) ; A=0.5(0.608+0.64)/2 = 0.312

For (0.5-1.0) ; A=0.5(0.64+0.608)/2 = 0.312
For (1.0-1.5) ; A=0.5(0.608+0.288)/2 = 0.224
For (1.5-2.0) ; A=0.5(0.228+0.096)/2 = 0.096
For (2.0-2.5) ; A=0.5(0.096+0.032)/2 = 0.032
For (2.5-3.0) ; A=0.5(0.032+0.032)/2 = 0.016
For (3.0-3.5) ; A=0.5(0.032+0)/2 = 0.008
5

E ( t ) dt=0.312+ 0.312+ 0.224+0.096+ 0.032+ 0.016+0.008=1

0

tm =

t E ( t ) dt=5 (1 )=5
0

18

9.0 DISCUSSION
This experiment was conducted by using SOLTEQ Tubular Flow Reactor model:
BP 101 to examine the effect of a pulse input and step change in a tubular reactor
and also to construct the residence time distribution (RTD) function for tubular flow
reactor. The experiment was run at flow rate 700mL/min. At constant conductivity of
solution, the conductivity of inlet and outlet of solution were recorded while running
the experiment. The flow through the vessel in tubular reactor is continuous and
usually at steady state.
From experiment 1 which is pulse input in a tubular flow reactor, the reaction was
flow at constant flow rate 700mL/min. The outlet conductivity is keep changing until it
reach 0.0 mS/cm at time 3.5 minutes to 5 minutes. It can be shown in graph 1, outlet
conductivity versus time, the highest conductivity is 2 mS/cm at minutes 0.5 and
suddenly steeply decrease from 1.9 mS/cm to 0.1 mS/cm at minutes 1 to 2.5. Based
on this result, the experiment is considered succeed since the result is not differ from
the theory where the conductivity is reaching zero at time of 3.5 minutes.
From experiment 2 which is step change input in a tubular flow reactor, the outlet
flow rate increase sharplyfrom 0 mS/cm to 2.7mS/cm at time of 2 minutes and kept
constant at 2.8 mS/cm from time of 3 to 5 minutes. This is shown in graph 3. From
both graph 1 and 2, it can be seen the differences between both graph where graph 3
is in increase smoothly while graph 1 decrease into a constant value.
In order to achieve second objectives, the residence time distribution is plotted
based on exit time,E(t) versus time,t. From the graph, it can be concluded that the
residence time distribution is depends on the outlet conductivity. From graph 2, in
experiment1, E(t) decreases over time and remain constant at 0mS/cm at 3.5 to 5
minutes. The residence time distribution calculated is 5.000 minutes. Besides, there
are three data had been obtained and calculated which are mean residence time, t m ,
variance (second moment),

2 ,

and skewness third moment, s3 which their values

are 1.1728, 42.608 and -8.9953 respectively. The skewness give negative value and
it is called negative skew.

19

Compare to experiment 2, graph 4 shows E(t) increase linearly against time from
0.5 to 5 minutes. The total residence time t m , variance (second moment),

and

skewness third moment, s3 calculated are 4.931x10-2, 0.186 and 0.778. The
skewness give the positive value and it is called positive skew, which is differ from
experiment 1.

10.0 CONCLUSION
The experiment was running to to examine the effect of a pulse input and step
change in a tubular reactor and also to construct the residence time distribution
(RTD) function for tubular flow reactor. The inlet and outlet conductivity for pulse input
after 3.5 minutes remains constant which are 0.2mS/cm and 0.0mS/cm. The outlet
conductivity, C(t) that had been calculated for pulse input is 3.125 and for step
change is 75.2. The distribution of exit time, E(t) is calculated for each 30 seconds
until 5 minutes interval. The total E(t) for pulse input and step change are 2.304 and
1. In pulse input, the mean residence time,t m is 1.1728 and total residence time in
step change is 4.931x10-2 . The variance (second moment),

2 ,

and skewness

third moment, s3 are also calculated which are 42.608 and -8.9953 in pulse input
while 0.186 and 0.778 in step change. The graph for outlet conductivity, C(t) against
time and distribution exit time, E(t) against time are plotted. The graph plotted shows
that exit time, E(t) is depends on the value of C(t), same as the theory. The
experiments are considered success as the objectives are achieve.

20

11.0 RECOMMENDATION
There are a few recommendations and preacutions that need to be taken
during conducting this experiment in order to get an accurate

and success

results.Firstly, do start-up and shut-down experiment everytime conduct the reactor to

make sure there are no left over in the chamber. Secondly, make sure the reactor
does not have any leaks and valve is closed and opened as needed, controlled the
valves carefully and slowly when adjusting the flowrate. This is to ensure the
stabilization of flowrate and the experiment can be run smoothly. This experiment
also should be conducted at the stable and unshaken place.

12.0 REFFERENCE
[1] http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm
http://www.neduet.edu.pk/Chemical/PDF/CHEMICAL%20REACTION
%20ENGINEERING%20LAB.pdf

(Retrieved on 23/3/16)

[2]http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm

(Retrieved

on 23/3/16)
[3] www.che.utah.edu/~ring/.../Hovorka&Kendall.pdf

(Retrieved on 23/3/16)

[4] http://pubs.acs.org/doi/abs/10.1021/ie0006716?journalCode=iecred

(Retrieved

on 23/3/16)
[5] ijsae.in/ijsaeems/index.php/ijsae/article/download/1056/727.pdf

(Retrieved on

23/3/16)

21

13.0 REFERENCE

(a)

(b)
Figure 2: (a) and (b) are SOLTEQ Tubular Flow Reactor model: BP 101

22