ABSTRACT

This experiment has been conducted on 5th April 2013 at Pilot Plant
Laboratory, UiTM Shah Alam. The experiment is conducted to achieve the
objective that has been considered which is to examine the effect of pulse
input and step change input in tubular flow reactor and to construct the
residence time distribution function by using tubular machine. Based on
the experiment, two experiment were conducted which is pulse input
experiment and step change input experiment. In the pulse input
experiment, the flow rate was set up at 700 m3 s-1 and let it for one minute
before reading taken every 30 seconds until the conductivity reading is
0.0. in the other hand, the step change input experiment, the conductivity
were observe every 30 seconds until the reading at Q2 is constant for 3
times.

INTRODUCTION
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. Flow in tubular reactors can be laminar , as with
viscous fluids in small-diameter tubes, and greatly deviate from ideal plugflow behavior, or turbulent, as with gases.
There are tubular flow reactors applications which arer:

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions

In an ideal plug flow reactor, a pulse of tracer injected at the inlet would
not undergo any dispersion as it passed through the reactor and would
appear as a pulse at the outlet. The degree of dispersion that occurs in a
real reactor can be assessed by following the concentration of tracer
versus time at the exit. This procedure is called the stimulus-response
technique.
High temperature reactions Residence Time Distribution (RTD) analysis
is a very efficient diagnosis tool that can beused to inspect the
malfunction of chemical reactors. Residence time distributions are
measured by introducing a non-reactive tracer into the system at the inlet.
The concentration of the tracer is changed according to a known function
and the response is found by measuring the concentration of the tracer at
the

outlet.

The

selected

tracer

should

not

modify

the

physical

characteristics of the fluid (equal density, equal viscosity) and the

introduction of the tracer should not modify the hydrodynamic conditions.
In general, the change in tracer concentration will either be a pulse or a
step.
The residence time distribution of a real reactor deviated from that of
an ideal reactor, depending on the hydrodynamics within the vessel. A
non-zero variance indicates that there is some dispersion along the path of
the fluid, which may be attributed to turbulence, a non-uniform velocity
profile, or diffusion. If the mean of the
expected time

curve arrives earlier than the

it indicates that there is stagnant fluid within the vessel. If

the residence time distribution curve shows more than one main peak it
may indicate channeling, parallel paths to the exit, or strong internal
circulation.

OBJECTIVES

To examine the effect of a pulse input and step change input in a

tubular flow reactor.

To construct a residence time distribution (RTD) function for the
tubular flow reactor.

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
small-diameter 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 neglected. In that case, the batch
reactor time and the residence-time would both be equal to the spacetime.
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 log-log 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.
PROCEDURE
Experiment 1: Pulse Input in a Tubular Flow Reactor
1. The general start-up procedures as in Section 4.1 is performed.
2. Valve V9 is opened and pump P1 is switch on.

3. Pump P1 flow controller is adjusted to give a constant flow rate of

de-ionized water into the reactor R1 at approximately 700 ml/min at
Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until
the inlet (Ql-01) and outlet (Ql-02) conductivity values are stable at
low levels. Both conductivities values are recorded.
5. Valve V9 is closed and pump P1 is switch off.
6. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
7. Pump P2 flow controller is adjusted to give a constant flow rate of
salt solution into the reactor R1 at 700 ml/min at Fl-02.
8. Let the salt solution to flow for 1 minute, then reset and restart the
timer. This will start the time at the average pulse input.
9. Valve V11 is closed and pump P2 is switch off. Then, open valve V9
quickly and pump P1 is switch on.
10.
Make sure that the de-ionized water flow rate is always
maintained at 700 ml/min by adjusting P1 flow controller.
11.
Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at
regular intervals of 30 seconds is start recorded.
12.
The conductivity values is continue recording until all readings
are almost constant and approach the stable low level values.

Experiment 2: Step Change Input in a Tubular Flow Reactor

1. The general start-up procedures as in Section 4.1 is performed.
2. Valve V9 is opened and pump P1 is switch on.
3. Pump P1 flow controller is adjusted to give a constant flow rate of
de-ionized water into the reactor R1 at approximately 700 ml/min at
Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until
the inlet (Ql-01) and outlet (Ql-02) conductivity values are stable at
low levels. Both conductivities values are recorded.
5. Valve V9 is closed and pump P1 is switch off.

6. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
7. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at
regular intervals of 30 seconds is start recorded.
8. The conductivity values is continue recording until all readings are
almost constant.

A P PA R AT U S A N D M AT E R I A L S

Tu b u l a r fl o w re a c t o r
Deionized water
S o d i u m h y d r ox i d e
Ethyl acetate

RESULTS AND CALCULATIONS

Experiment 1: Pulse input in Tubular Flow Reactor
Flow rate : 700mL/min
Input type : Pulse input

Time (min)
0.0
0.5
1.0
1.5

Conductivity (mS/cm)
Inlet
Outlet
0.0
0.0
0.3
0.0
0.0
0.2
0.0
1.8

2.0
2.5
3.0
3.5
4.0

0.0
0.0
0.0
0.0
0.0

2.1
1.1
0.1
0.0
0.0

Outlet conductivity vs Time

2.5
2

Outlet COnductivity (mS/cm)

1.5

Conductivity (mS/cm)

Conductivity (mS/cm)
Outlet

0.5
0
05
Time(min)

C ( t ) dt

= Area under the graph

Area = (

t1

t2

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

For time (1.0-1.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (1.5 1.0)

0.2+1.8
2

= 0.5 g .min

= (2.0 1.5)

1.8+2.1
2

= 0.975 g .min

For time (1.5 2.0) minutes

Area = ( t 2 t 1
m

E (t 1+t 2)
2

For time (2.0 2.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (2.5 2.0)

2.1+1.1
2

= 0.8 g .min

m3

= (3.0 2.5)

1.1+0.1
2

= 0.3 g .min

m3

For time (2.5 3.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

So the total area or

C ( t ) dt
0

g.min/m3
E (t)=

C (t)

C ( t ) dt
0

For t = 0, C(t) = 0.0

E(t)=0/2.575=0

For t = 0.5, C(t) = 0.0

E(t)=0.0/2.575=0
For t = 1.0, C(t) = 0.2
E(t)=0.2/ 2.575=0.07767

For t = 1.5, C(t) = 1.8

E(t)=1.8/2.575=0.69903
For t = 2.0, C(t) = 2.1
E(t)=2.1/2.575=0.81553

For t = 2.5, C(t) = 1.1

= ( 0.5+ 0.975 + 0.8 + 0.3) = 2.575

E(t)=1.1/2.575=0.42718

For t = 3.0, C(t) = 0.1

E(t)=0.1/2.575=0.038833

Time (min)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
For t = 3.5, C(t) = 0.0

Conductivity
Outlet
0.0
0.0
0.2
1.8
2.1
1.1
0.1
0.0
0.0

E(t)
0.0
0.0
0.07767
0.69903
0.81553
0.42718
0.038833
0.0
0.0

E(t)=0.0/2.575=0

For t = 4.0, C(t) = 0.0

E(t)=0.0/2.575=0

Residence time distribution (RTD) function for plug flow reactor

E(t) vs Time
1
0.8
0.6
E(t)

E(t) 0.4
0.2
0
0

0.5

1.5

2.5

3.5

4.5

Time(minutes)

For time (0 0.5)minutes = 0

For time (0.5 -1.0)minutes
Area = ( t 2 t 1

E (t 1+t 2)
2

= (1 0.5)

0.07767
2

= 0.019418

For time (1 1.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (1.5 1)

0.07767+ 0.69903
2

0.19418
For time (1.5 2.0 )minutes
Area = ( t 2 t 1

E (t 1+t 2)
2

= (2 1.5)

0.69903+0.81553
2

= 0.37864

= (2.5 2)

0.81553+0.42718
2

= 0.310678

For time (2.0 2.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

For time (2.5 -3.0) minutes

Area = ( t 2 t 1

E ( t 1 +t 2 )
2

= (3 2.5)

0.42718+0.038833
=0.116503
2

= (3.5- 3)

0.038833
2

For time (3 -3.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= 0.0097083

E ( t ) dt
0

= Total area under the graph = (0.019418 + 0.37864 +0.310678

+ 0.116503 + 0.0097083 =0.834947

Residencetime , t m=

tE ( t ) dt
0

time

Outlet

(min)

conducti

E(t)

= 4(0.834947)= 3.339788

tE(t)
(ttm)2E(t)dt

vity

(mS/cm)
0
0
0
0
0
0.5
0.0
0.0
0.0
0
1
0.2
0.077670
0.077670
0.425213
1.5
1.8
0.699903
1.049855
2.369046
2
2.1
0.815530
1.631060
1.463902
2.5
1.1
0.427180
1.067950
0.301266
3
0.1
0.038833
0.116499
0.004483
3.5
0.0
0.0
0.0
0
4
0.0
0.0
0.0
0

=3.9430 =4.60425 =-7.56929

=2.05912 34
7

Mean residence time,

tE ( t ) dt =

t m=

3.943034

Second moment, variance ,

= 4.604257

(ttm )2
0

E(t) dt

(ttm)3E(t)dt
0
0
-0.994908
-4.358542
-1.961319
-0.252999
-0.001523
0
0

s=

Third moment, skewness,

(ttm )3

3
2

1
=

(2.145753)

3
2

E(t) dt

-7.56929) = -2.40816

Experiment 2: Step Change Input in a Turbular 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

Conductivity (mS/cm)
Inlet
outlet
0.0
0.0
2.7
0.0
2.8
0.0
2.8
0.0
2.8
0.0
2.7
1.3
2.7
1.6
2.6
1.6
2.6
1.6

Outlet Conductivity vs Time

1.8
1.6
1.4
1.2
1

Conductivity (mS/cm)
outlet

Outlet conductivity (mS/cm) 0.8

0.6
0.4
0.2
0
0 5
Time(min)

Conductivit
y (mS/cm)

C(t)

E(t)

tm

s3

Inlet

Outlet

Cit

Ci(t)/Ci(
t)

t*E(t)/
C i t

(t - tm) 2 *
E(t)/
C i t

(t - tm) 3 *
E(t)/
C i t

0.00

0.0

0.0

0.00000

0.00000

0.00000

0.00000

0.50

2.7

0.0

0.00000

0.00000

0.00000

0.00000

1.00

2.8

0.0

0.00000

0.00000

0.00000

0.00000

1.50

2.8

0.0

0.00000

0.00000

0.00000

0.00000

2.00

2.8

0.0

0.0000

0.0000

0.0000

0.0000

2.50

2.7

1.3

0.000
0
0.000
0
0.000
0
0.000
0
0.000
0
3.25

0.16209

0.02021

0.049713

0.12328

Time
(min)

3.00

2.7

1.6

4.80

0.23940

0.03582

0.104910

0.31097

3.50

2.6

1.6

5.6

0.27930

0.04876

0.165923

0.57264

4.00

2.6

1.6

6.4

0.31920

0.06368

0.246677

0.84963

=20.
05

=1.0008

=0.1684
7

=
0.567223

=1.8565
2

Residence time distribution (RTD) function for plug flow reactor

E(t) vs Time
0.35
0.3
0.25
0.2

E(t)

E(t) 0.15
0.1
0.05
0
0

0.5

1.5

2.5

Time(min)

SAMPLE OF CALCULATION

C (t)dt=C i t=Area
0

So based on the table, Area is 20.05m2

Example of calculation at t=0.00min
t m=

t E( t)
Area

t m=

2.50 0.16209
20.05

3.5

4.5

t m=0.02021

2=

2
( t t m ) E(t )

Area

( 2.500.02021 )2 0.16209
20.05

2=0.049713

s=

3
( tt m ) E(t)

Area

( 2.500.02021 )3 0.16209
s=
20.05
3

s 3=0.12328

DISCUSSION
Firstly, the objective that need to be achieve for this tubular reactor
experiment is 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 the tubular flow reactor at the end of the experiment. The
experiment was run at the 700 mL/min of flowrate. While the experiment
is running, the conductivity for the inlet and outlet of the solution had

been recorded at the period of time where until the conductivity of the
solution is constant.
For a tubular reactor, the flow that throught the vessel is continuous,
usually at the steady state and also configured thus the conversion of the
chemicals and other dependent variables are functions of position within
the reactor rather than of time.
For this experiment, we are examined the effects of flow for two
types of reaction which are in pulse input and step change. The flowrate of
solution is kept constant at 700 ml/min. For this types of experiments, the
graph of outlet conductivity versus times had been plotted. Based on
graph of pulse input, the outlet conductivity that had been plotted is 2.1
mS/cm at time of 2 minutes which are the highest value. After that, the
conductivity is decrease within the time and comes to be constant at the
time of 3.5 minutes. From the result, it showed that it result was not differ
from the theory that recorded that the conductivity is reaching zero at
time of 4 minutes. Thus, the experiment 1 is succeed.
In addition, for the graph of step change the outlet conductivity is
increase within the time by started at time of 2.0 minutes which it inlet
conductivity is 2.8 mS/min and then undergoes some increament until at
minutes 4.0 which the outlet conductivity is 1.6 mS/min. There are
differences between both of the graph where the outlet conductivity for
step change is increase smoothly compare to pulse input where the outlet
conductivity is increase at the some period of times and then it become
decrease into the constant value.
Next experiment, to construct the residence time distribution (RTD)
function for the tubular flow reactor for pulse input and also step change.
The residence time distribution is plotted based on exit time (E(t)) versus
time from the data that had been recorded in the table. From the graph
plotted, it almost same with the graph that are stated at the theory. From
the graph, it can be concluded tha the residence time distribution is
depends on the outlet conductivity.

For the pulse input graph, the residence time distribution calculated
is 3.339788 minutes. besides, there are 3 data that had been obtained and
calculated which are mean residence time,

tm

variance (second moment),2

and skewness (third moment),s3 that recorded 3.943034, 4.604257 and

-2.40816 respectively. The skewness for the pulse input give a negative
value and it called negative skew.
Compare ot the step change, the graph almost same to the outlet
conductivity versus time which the residence time distribution (RTD) is
increase within the time. For the step change, the mean residence time
distribution that calculated is 0.02021 minutes. The other 2 data are also
need to be calculate which are variance (second moment), 2 and
skewness (third moment), s3 are 0.049713 and 0.12328 respectively. The
skewness give a positive value and it called positive skew compare to
pulse input.

C O N C LU S I O N

From the experiment, we able to examine the effect of the pulse

input and step change in a tubular flow reactor and we also can
differentiate both of the effect. Besides, we also able to construct the
residence time distribution (RTD) function for the tubular flow reactor.
The conductivity for inlet and outlet after 3 minutes for pulse input
are 0.00 mS/min and 0.1 mS/min while for the step change is 2.7 mS/min
and 1.6 mS/min respectively. The outlet conductivity, C(t) that had been
calculated for pulse input is 2.575 and for step change is 20.05. The
distribution of exit time, E(t) is calculated for each 30 second until 4
minutes interval. The sum of E (t) for pulse input and step change are
2.05912 and 1.0008 respectively. The mean residence time, t m for pulse
input is 3.943034 minutes and step change is 0.16847 minutes.
The variance, 2 and skewness, s3 are also calculated. For pulse input
are 4.604257 and -2.4081 while for step change are 0.567223 and
1.85652. graph for outlet conductivity, C (t) against time and distribution
of exit time, E (t) against time are plotted. The graph plotted almost the
same as the theory which stated that exit time, E (t) is depends on the
value of C (t).

R E C O M M E N D AT I O N
I.

Each experiment we must do the start-up and shut-down experiment

II.
III.

first in order to make sure there are no left over in the chamber.
Open and close the valve carefully according to the procedure given.
The experiment should be conducted at the stable and unshaken

IV.

place.
Make sure there are no leakages at the equipment.

REFERENCES:
(K. G. Denbigh, Chemical Reactor Theory: An Introduction, 41-45)

(Artin
hatzikioseyian,
Emmanouela
Remoundaki,http://www.metal.ntua.gr/~pkousi/elearning/bioreactors/page_07.htm
http://www.neduet.edu.pk/Chemical/PDF/CHEMICAL%20REACTION
%20ENGINEERING%20LAB.pdf

Turbular

Reactor.

(n.d.).

Retrieved

April

2013,

from

Scrib:

http://www.scribd.com/doc/95675475/Turbular-Reactor

Wikipedia. (n.d.). Retrieved April 2013, from Plug Flow Reactor

Model: http://en.wikipedia.org/wiki/Plug_flow_reactor_model

http://www.metal.ntua.gr/~pkousi/e-

learning/bioreactors/page_07.htm
http://en.wikipedia.org/wiki/Residence_time_distribution

APPENDICES: