1) ABSTRACT

The experiment is conducted to examine the effect of a pulse input and step change input
in a tubular flow reactor as well as to construct a residence time distribution (RTD) function for
the tubular flow reactor. Based on the experiment, there were two experiments conducted which
is pulse input experiment and step change input experiment. For pulse input experiment, the flow
rate was set up at 700 m3 s-1 and let the salt solution to flow for one minute before reading taken
every 30 seconds until the conductivity reading is 0.0. In step change input experiment, the
conductivity was observed every 30 seconds until the reading at Q2 is constant for 3 times. The
calculation steps of all criterion evaluated is shown in calculation section and the results is
simplified in Table.

2) 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. Turbulent flow reactor generally is preferred to
laminar flow because mixing and heat transfer are improved.
There are tubular flow reactors applications which are:

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions

High temperature reactions Residence Time Distribution (RTD) analysis is a very efficient
diagnosis tool that can beused to inspect the malfunction of chemical reactors. It also useful in
the estimation of effluent properties and in modeling reactor behavior.
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 nonuniform 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.

3) OBJECTIVE

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.

4) THEORY

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 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 space-time.
Using the result of experiment, the equation below is used apply equation 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 obtained 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 operates
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) PROCEDURE
4

Experiment 1: Pulse Input in a Tubular Flow Reactor

1. The general start-up procedure 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.
5

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.

6) APPARATUS

SOLTEQ Tubular flow reactor equipment

Deionized water
Sodium hydroxide
Ethyl acetate

7) RESULT

RESULTS AND CALCULATIONS

Experiment 1: Pulse input in Tubular Flow Reactor
Flow rate: 700 mL/min
Input type : Pulse Input
6

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

2.9
2.9
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0

0.0
0.3
1.7
2.0
2.0
2.1
2.2
2.2
2.3
2.3
2.3

Outlet conductivity against Time

12
10
8
Outlet conductivity(mS/cm)

6
4
2
0
0

Time(min)

10 12

C ( t ) dt
0

Area = (

t1

= Area under the graph

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)

1.7+0.3
2

3
= 0.925g .min m

= (2.0 1.5)

2.0+2.0
2

= 1.00 g .min m

= (2.5 2.0)

2.1+2.0
2

= 1.1025 g .min m

= (3.0 2.5)

2.1+2.2
2

3
= 1.075 g .min m

For time (1.5 2.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

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

So the total area or

C ( t ) dt
0

= (0.925+1.00+1.1025+1.1075) = 4.135 g.min/m3

E (t)=

C (t)

C ( t ) dt
0

For t = 0, C(t) = 0.0

E(t)=0/ 4.135=0
For t = 0.5, C(t) = 0.3
E(t)=0.3/4.135=0.0726

For t = 1.0, C(t) = 1.7

E(t)=1.7/4.135=0.4111
For t = 1.5, C(t) = 2.0
E(t)=2.0/4.135=0.4837

For t = 2.0, C(t) = 2.0

E(t)=2.0/4.135=0.4837
For t = 2.5, C(t) = 2.1
E(t)=2.1/4.135=0.5079

For t = 3.0, C(t) = 2.2

E(t)=2.2/4.135=0.5320
For t = 3.5, C(t) = 2.2
E(t)=2.2/4.135=0.5320

For t = 4.0, C(t) = 2.3

E(t)=2.3/4.135=0.5562
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
Outlet
0.0
0.3
1.7
2.0
2.0
2.1
2.2
2.2
2.3
2.3
2.3

E(t)=2.3/4.135=0.5562
For t = 5.0, C(t) = 2.3
E(t)=2.3/4.135=0.5562

10

E(t)
0.0
0.0726
0.4111
0.4837
0.4837
0.5079
0.5320
0.5320
0.5562
0.5562
0.5562

For t = 4.5,
C(t) = 2.3

E(t) against Time

12
10
8
E(t)

6
4
2
0
0

10

12

Time(min)

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)

0.0726
2

= 0.0182

For time (1 1.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (1.5 1)

0.0726+ 0.4111
2

= 0.1209

For time (1.5 2.0 )minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (2 1.5)

0.4111+0.4837
2

= (2.5 2)

0.4837+ 0.5079
2

= 0.2237

= 0.2479

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

11

Area = ( t 2 t 1

E ( t 1 +t 2 )
2

= (3 2.5)

0.5079+0.5320
=0.2600
2

= (3.5- 3)

0.5320+0.5320
2

= 0.2660

= (4-3.5)

0.5320+0.5562
2

= 0.2721

= (4.5-4)

0.5562+0.5562
2

= 0.2781

= (5-4.5)

0.5562+0.5562
2

= 0.2781

For time (3 -3.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

For time (3.5 -4.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

For time (4.5-4.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

For time (5.0-4.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

E ( t ) dt
0

= Total area under the graph =

(0.0182+0.1209+0.2237+0.2479+0.2600+0.2660+0.2721+0.2781+0.2781)= 1.965

Residencetime , t m=

tE ( t ) dt

= 5(1.965)= 9.825

Time

Outlet

(min)

conductivity

0
0.5
1
1.5
2

(mS/cm)
0.0
0.3
1.7
2.0
2.0

E(t)

tE(t)
(t-tm)2E(t)dt

0.0
0.0726
0.4111
0.4837
0.4837

0
0.0363
0.4111
0.7256
0.9674
12

0
6.3130
32.0167
33.5231
29.6173

(t-tm)3E(t)dt
0
-58.8685
-282.5476
-279.0801
-231.7550

2.5
3
3.5
4
4.5
5
=4.6916

2.1
2.2
2.2
2.3
2.3
2.3
=14.3769

0.5079
0.5320
0.5320
0.5562
0.5562
0.5562
=222.3780

1.2698
1.596
1.862
2.2248
2.5029
2.781
=-1612.005

27.2517
24.7809
21.2830
18.8722
15.7714
12.9487

-199.6186
-169.1296
-134.6149
-109.9306
-83.9827
-62.4774

Mean residence time,

tE ( t ) dt =

t m=

14.3769

Second moment, variance ,

(ttm )2

E(t) dt

= 222.3780
3

Third moment, skewness,

s=

(ttm )3

3
2

1
=

3
2

(14.9123)

E(t) dt

-1612.005) = -654.9149

Experiment 2: Step Change Input in a Turbular Flow Reactor

Flow rate

= 700 mL/min

Input type : Step change

Time (min)
0.0

Conductivity (mS/cm)
Inlet
0.1
13

Outlet
0.0

0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
12.0
12.5

2.4
2.8
2.9
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0

Outlet conductivity against Time

0.12
0.1
0.08
Outlet conductivity(mS/cm) 0.06
0.04
0.02
0
0 2 4 6 8 10 12 14
Time(min)

14

0.2
2.1
2.0
0.5
1.5
2.1
2.3
2.3
2.5
2.5
2.6
2.7
2.7
2.8
2.8
2.9
2.9
3.0
3.1
3.0
3.1
3.1
3.2
3.2
3.2

Time
(min)

Conductivity
(mS/cm)

C(t)

E(t)

s3

Inlet

Outlet

Cit

Ci(t)/Ci(t)

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

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

0.0
0.5

0.1
2.4

0.0
0.2

0
0.575

0
0.0063

0
1004.0676

1.0

2.8

2.1

1.1025

0.0657

10444.7785

6
-4.2 10

1.5

2.9

2.0

0.625

0.0625

9911.1482

6
-3.9 10

2.0

3.0

0.5

0.500

0.0156

243467.61

5
-9.8 10

2.5

3.0

1.5

0.900

0.0469

7400.0196

6
-2.9 10

3.0

3.0

2.1

1.100

0.0657

10340.2579

-4.1 10

3.5

3.0

2.3

1.150

0.0719

11287.5448

6
-4.5 10

4.0

3.0

2.3

1.200

0.0719

11259.0746

-4.5 10

4.5

3.0

2.5

1.250

0.0782

12214.688

6
-4.8 10

5.0

3.0

2.5

1.275

0.0782

12183.8016

6
-4.8 10

5.5

3.0

2.6

1.325

0.0813

12634.7208

-5.0 10

6.0

3.0

2.7

1.350

0.0844

13083.2365

6
-5.2 10

6.5

3.0

2.7

1.375

0.0844

13050.0278

-5.1 10

7.0

3.0

2.8

1.400

0.0876

13510.3915

6
-5.3 10

7.5

3.0

2.8

1.425

0.0876

13476.0112

6
-5.3 10

8.0

3.0

2.9

1.450

0.0907

13917.3504

6
-5.4 10

8.5

3.0

2.9

1.475

0.0907

13881.8442

6
-5.4 10

9.0

3.0

3.0

1.525

0.0938

14319.6334

-5.6 10

9.5

3.0

3.1

1.525

0.0969

14755.0471

6
-5.8 10

10.0

3.0

3.0

1.525

0.0938

14246.4283

-5.6 10

10.5

3.0

3.1

1.550

0.0969

14679.5196

6
-5.7 10

11.0

3.0

3.1

1.575

0.0969

14641.8285

6
-5.7 10

11.5

3.0

3.2

1.600

0.1001

15086.4706

-5.9 10

12.0

3.0

3.2

1.600

0.1001

15047.6349

6
-5.8 10

12.5

3.0

3.2

1.600

15008.8493

-5.8 10

=540842

=6.1

15

0.1001

-4.0 10

Residence time distribution (RTD) function for plug flow reactor

8) DISCUSSION

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
through 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.
The experiment is conducted to examine the effects of flow for two types of reaction
which are in pulse input and step change. The flow rate of solution is kept constant at 700
ml/min. In this experiment, the graph of outlet conductivity versus times had been plotted. Based
on graph of pulse input, the outlet conductivity that had been plotted is 2.3 mS/cm at time of 4
minutes which are the highest value. After that, the conductivity is increased within the time and
comes to be constant at the time of 4 minutes. From the result, it showed that it result was differ
from the theory that recorded that the conductivity is not reaching zero but keep increased until
the value constant .There are some error occurs while conducting the experiment. However, the
experiment can be said successfully conducted because the objective of this experiment is
achieved.
In addition, for the graph of step change the outlet conductivity is increase within the
time by started at time of 11.5 minutes which it inlet conductivity is 3.2 mS/min .There are
differences between both of the graph where the outlet conductivity for step change is increase
smoothly and the time also increase until the value of conductivity achieve constant compare to
pulse input.

16

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 the residence time distribution is depends on the outlet conductivity.
For the pulse input graph, the residence time distribution calculated is 9.825 minutes.
Besides, there are 2 data that had been obtained and calculated which are variance (second
moment),2 and skewness (third moment),s3 that recorded 222.3780 and 1612.005 respectively.
The skewness for the pulse input give a negative value and it called negative skew.
Compare to 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 0.3541 minutes. The other 2 data are also need
to be calculate which are variance (second moment), 2 and skewness (third moment), s3 are
7
540842 and 6.1 10

respectively. The skewness also give negative value . There are some

error occurs while conducting the experiment. However, the experiment can be said successfully
conducted because the objective of this experiment is achieved.

9) CONCLUSION

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. The flow rate of both
experiments was kept constant at 700 ml/min and deionized water "as used .Besides, we also
able to construct the residence time distribution (RTD) function for the tubular flow reactor.
A 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
17

time, E (t) is depends on the value of C (t). The experiment was considered a success as all
objectives were achieved.

10) RECOMMENDATION

A few recommendations are suggested on the techniques employed during the experiment.
Firstly, before run the experiment, students should consult the experiment first with assistant lab.
In each experiment, students must do the start-up and shut-down experiment 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. Besides that, the experiment should be conducted at the stable and unshaken
place. Make sure there are no leakages at the equipment as well as make sure that the time taken
to let the conductivity is 30 seconds and the flow rate is maintained a 700 ml/min.

11) REFERENCE

(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

18

Turbular

Reactor.

(n.d.).

Retrieved

April

2013,

from

Scrib:

Reactor

Model:

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

Wikipedia.

(n.d.).

Retrieved

April

2013,

from

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

12) APPENDICES

19

Plug

Flow