1) ABSTRACT

A tubular reactor is a vessel through which flow is continuous, usually at steady state, and
configures so that conversion of the chemicals and other dependent variables are functions
of position within the reactor rather than of time. This experiment is conducted to achieve
the objective that has been considered which are 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 m 3 s-1 and let it for one minute before
reading taken every 30 seconds until the conductivity reading is 0.0. On 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. Result show that when the outlet conductivity
increases at some period of time, it will then decrease into a constant value. In conclusion,
both experiment had been done successfully, abiding stated theories.

2) INTRODUCTION

A tubular reactor is a vessel through which flow is continuous, usually at steady state, and
configures 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 plug-flow
behaviour, or turbulent, as with gases. There are tubular flow reactors applications which
are large-scale reactions, fast reactions, homogeneous or heterogeneous reactions,
continuous production, and high-temperature reactions.
As for 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 the
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 very
efficient diagnosis tool that can be used 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 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.

3) OBJECTIVE

3.1

Experiment 1

To examine the effect of a pulse input in a tubular flow reactor

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

3.2

Experiment 2

To examine the effect of a step change input in a tubular flow reactor

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

4) 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 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 obtained from the intercept and slope of the appropriate log-log
plot. This approach is 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

4

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) APPARATUS AND MATERIAL

Tubular flow reactor

Deionized water
Sodium chloride solution (NaCl)

6) PROCEDURE

6.1

General Start-Up Procedure

1. All valves are ensured closed except for valve V7.
2. The following solutions are prepared:
Tank B1: Deionized water
Tank B2: 0.05M sodium chloride solution (NaCl).
3. The power for control panel was turned on.
4. Water jacket B4 and pre-heater B5 was filled with clean water. Valves V13 and V8
were opened. Pump P3 was switched on to circulate the water through pre-heater
B5.
5. Stirrer motor M1 was switched on and the speed was set to about 200 rpm.
6. Valves V2 and V10 were opened. Pump P1 was switched on. P1 was adjusted to
flowrate of 700 mL/min at flow meter FI-01. Valve V10 was closed and pump P1
was switched off.
7. Valves V6 and V12 were opened. Pump P2 was switched on. P2 was adjusted to
flowrate of 100 mL/min at flow meter FI-02. Valve V12 was closed and pump P2
was switched off.
8. The unit is ready for experiment.

6.2

Experimental procedure
5

6.2.1

Experiment 1: Pulse Input in a Tubular Flow Reactor

1. The general start-up procedure was performed as in 6.1.

2. Valve V9 was opened and pump P1 was switched on.
3. Pump P1 flow controller was adjusted to give a constant flow rate of deionized
water into the reactor R1 at approximately 700 mL/min at F1-01.
4. The deionized water continued to flow through the reactor until the inlet (QI-01)
and outlet (QI-02) conductivity values were stable at low levels. Both conductivity
values were recorded.
5. Valve V9 was closed and pump P1 was switched off.
6. Valve V11 was opened and pump P2 was switched on. The timer was set
simultaneously.
7. Pump P2 was flow controller was adjusted to give a constant flow rate of salt
solution into the reactor R1 at 700 mL/min at FI-02.
8. The salt solution was allowed to flow for 1 minute and the timer was reset and
restarted.
9. Valve V11 was closed and pump P2 was switched off. Valve V9 was quickly
opened and pump P1 was switched on.
10. The deionized water flowrate was made sure always maintained at 700 mL/min by
adjusting P1 flow controller.
11. Both the inlet (QI-01) and outlet (QI-02) conductivity values were recorded at
regular intervals of 30 seconds.
12. Conductivity values were recorded until all readings were constant and approach
stable low level values.

6.2.2

Experiment 2: Step Change Input in a Tubular Flow Reactor

1. The general start-up procedure was performed as in 6.1.

2. Valve V9 was opened and pump P1 was switched on.
3. Pump P1 flow controller was adjusted to give a constant flow rate of deionized
water into the reactor R1 at approximately 700 mL/min at FI-01.
4. The deionized water was allowed to flow through the reactor until the inlet (QI-01)
and outlet (QI-02) conductivity values are stable at low levels. Both conductivity
values were recorded.
5. Valve V9 was closed and pump P1 was switched off.
6. Valve V11 was opened and pump P2 was switched on. The timer was set
simultaneously.

7. Both the inlet (QI-01) and outlet (QI-02) conductivity values were recorded at
regular intervals of 30 seconds.
8. The conductivity values were taken down until all readings are almost constant.

6.3

General Shut-Down Procedure

1. Both pumps P1 and P2 were switched off. Valves V2 and V6 were closed.
2. The heaters were switched off.
3. Cooling water was kept to circulate through the reactor while the stirrer motor is
switched on to allow the water jacket to cool down to room temperature.
4. The power for the control panel was switched off.

7) RESULT AND CALCULATION

Experiment 1: Pulse Input in a Tubular Flow Reactor
Time
(min)

Conductivity (ms/cm)
Inlet
Outlet

0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5

0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0

Time, t

Outlet
Conductivity,
C(t)
0.0
1.7
2.0
2.1
0.7
0.2
0.0
0.0
0.0

0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5

C(t)

E(t)

Tm
(min)

0.0
1.7
2.0
2.1
0.7
0.2
0.0
0.0
0.0

0.0
1.7
2.0
2.1
0.7
0.2
0.0
0.0
0.0

0.0000
0.4256
0.5007
0.5257
0.1752
0.0501
0.0000
0.0000
0.0000

E(t)

1.0000

tE(t)

0.0000
0.0000
0.4256
0.4256
0.5007
0.7511
0.5257
1.0514
0.1752
0.4380
0.0501
0.1503
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
Table 7.1 Result of experiment 1

(min)

0.7361

s3
(min3)

1.1776

(t-tm)2E(t)

(t-tm)3E(t)

0.0000
0.0000
0.1252
0.5257
0.3942
0.2004
0.0000
0.0000
0.0000

0.0000
0.0000
0.0626
0.5257
0.5913
0.4008
0.0000
0.0000
0.0000

Conductivity vs Time
2.5
2
1.5
Conductivity

Conductivity vs Time
1
0.5
0
0.5

1.5

2.5

3.5

4.5

Time

Figure 7.1 Graph of Conductivity vs Time

E(t) vs Time
0.6
0.5
0.4
E(t)

0.3

E(t) vs Time

0.2
0.1
0
0.5

1.5

2.5

3.5

Time

Figure 7.2 Graph of E(t) vs Time

4.5

Experiment 2: Step Change Input in Tubular Flow Reactor

Time
(min)
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

Conductivity
(ms/cm)
Inlet
Outlet
0.0
0.0
2.8
0.0
3.0
0.0
3.1
0.0
3.1
0.8
3.1
1.8
3.1
1.9
3.1
1.9
3.1
1.9
3.1
2.0
3.1
2.0
3.1
2.0
3.1
2.0

t (min)

C (t)

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

0.0
0.0
0.0
0.0
0.8
1.8
1.9
1.9
1.9
2.0
2.0
2.0
2.0

E(t) (min-1)

C(t)

E(t)

0.0
0.0
0.0
0.0
0.8
1.8
1.9
1.9
1.9
2.0
2.0
2.0
2.0

0.0000
0.0000
0.0000
0.0000
0.1000
0.2250
0.2375
0.2375
0.2375
0.2500
0.2500
0.2500
0.2500

tE(t)

tm
(min)

4.1334

(t-tm)

0.0000
0.0000
-4.1334
0.0000
0.0000
-3.6334
0.0000
0.0000
-3.1334
0.0000
0.0000
-2.6334
0.1000
0.2000
-2.1334
0.2250
0.5625
-1.6334
0.2375
0.7125
-1.1334
0.2375
0.8313
-0.6334
0.2375
0.9500
-0.1334
0.2500
1.1250
0.3666
0.2500
1.2500
0.8666
0.2500
1.3750
1.3666
0.2500
1.500
1.8666
Table 7.2 Result of experiment 2

10

s3

(min2)

(min3)

1.4051

-0.4096

(t-tm)2E(t)

(t-tm)3E(t)

0.0000
0.0000
0.0000
0.0000
0.4551
0.6003
0.3051
0.0953
0.0042
0.0336
0.1877
0.4669
0.8710

0.0000
0.0000
0.0000
0.0000
-0.9710
-0.9805
-0.3458
-0.0604
-0.0006
0.0123
0.1627
0.6381
1.6259

Conductivity vs Time
2.5
2
1.5
Conductivity

Conductivity vs Time
1
0.5
0
0

0.5

1.5

2.5

3.5

4.5

5.5

Time

Figure 7.3 Graph of Conductivity vs Time

E(t) vs Time
0.3
0.25
0.2
E(t)

0.15

E(t) vs Time

0.1
0.05
0
0

0.5

1.5

2.5

3.5

4.5

Time

Figure 7.2 Graph of E(t) vs Time

11

5.5

Sample of calculation
Experiment 1: Pulse input in tubular flow reactor
Residence time distribution function, E (t)
N+1 = 9
N=8

C ( t ) dt = 3h [ C0 + 4 C1 + 2 C2 + 4 C3 + 2 C4 + .. + 4 CN-1 + CN ]
0

where, h =

h=

tN - t0
N

tN - t0
4.5 - 0
=
= 0.56
N
8

4.5

C ( t ) dt = 0.56
3
0

(0.0) + 4 ( 1.7 ) + 2 ( 2.0 ) + 4 ( 2.1 ) + 2 ( 0.7 ) + 4 ( 0.2 ) = 3.9947 g.min /m

+ 2(0)+ 4(0)+2(0)

At time = 0 minute, C (t) = 0.0

E (t) =

C(t )
2.75

C ( t ) dt
0

E (t) =

0.0
= 0.0
3.9947 mS.min /m

Mean residence time, tm

E ( t ) dx =
0

h
[ E0 + 4 E1 + 2 E2 + 4 E3 + 2E + .. + 4 EN-1 + EN ]
3

12

4.5

t m = tE ( t ) dt
0

0.56 (0.00) +4 ( 0.4256 ) + 2 ( 0.5007 ) + 4 ( 0.5257 ) + 2 ( 0.1752 ) +

3
4 ( 0.0501 ) + 2(0) + 4(0) + 2(0)

= 1.0000 min

Second moment, variance, 2

2 = ( t- t m )2 E(t) dt
0

4.5

2= ( t- t m ) 2 E ( t ) dt
0

2=

0.56 (0.0) +4 ( 0 ) + 2 ( 0.1252 ) + 4 ( 0.5257 ) + 2 ( 0.3942 ) +

3
4 ( 0.2004 ) + 2(0) + 4(0) + 2(0)

= 0.7361 min2

= 0.8580 min

Third moment, skewness, s3

tt m

1
( 0.56 ) [ 0+ 4 ( 0 ) +2 ( 0.0626 ) +4 ( 0.5257 ) +2 ( 0.5913 ) +4 ( 0.4008 )+ 2 ( 0 )+ 4 ( 0 )+ 2 ( 0 ) ]
3

= 0.9359 min3
1

( tt m )3 E ( t ) dt

3
2 0

1
=

0.8580

3
2

x(0.9359)

13

S3 = 1.1776 min3

Experiment 2: Step Change input in tubular flow reactor

Residence Time Distribution Function, E(t)
N + 1 = 13
N = 12
XN

C(t )dX
X0

t Nt

Where, h =

h=

h
3

[ C0 + 4 C 1+2 C 2+ 4 C 3+ 2C 4 ++ 4 C N 1+C N ]

t Nt 6.000.00
=
N
12
0

= 0.5

2. ves are achieved successfully . edure

6.00

[0+ 4 ( 0 ) +2 ( 0 ) + 4 ( 0 ) +2 ( 0.8 ) +4 (1.8 )+ 2 ( 1.9 ) + 4 ( 1.9 ) +2 ( 1.9 )+ 4 ( 2.0 )+2 ( 2.0 ) + 4 ( 2.0 ) +2 ( 2.0 )
C ( t ) dt= 0.5
3
0

=8 g min / m3
At time = 0.00 min, C(t) = 0.0
C (t)
E ( t ) = 6.00
C ( t ) dt
0

E ( t ) =

0.0
8

= 0.0000

14

Mean Residence Time, tm

E( t)dX
0

h
3

[ E0 +4 E1 +2 E 2+ 4 E3 +2 E4 + +4 EN 1+ EN ]

2.00

tm =

tE ( t ) dt
0

2. ves are achieved successfully . edure

6.00

[0+ 4 ( 0 ) +2 ( 0 ) + 4 ( 0 ) +2 ( 0.2 ) +4 ( 0.5625 ) +2 ( 0.7125 )+ 4 ( 0.8313 ) +2 ( 0.95 ) + 4 ( 1.125 ) +2 (1.25

tE ( t ) dt= 0.5
3
0

= 4.1334 min

Second moment, Variance,2

2 =

( ttm )2 E ( t ) dt
0

2
At t = 0.00 min and tm = 4.1334 min, ( ttm ) = (0.0000 4.1334)2 = 17.085

( ttm )2 E ( t ) dt
0

0.5
[0+ 4 ( 0 )+2 ( 0 ) + 4 ( 0 ) +2 ( 0.4551 ) +4 ( 0.6003 )+ 2 ( 0.3051 ) + 4 ( 0.0953 ) +2 ( 0.0042 )+ 4 ( 0.0336 )+ 2 ( 0.1877 )+
3

( ttm )2 E ( t ) dt
0

= 1.4051min

2 = 1.4051 min2
= 1.1854 min

15

Third moment, Skewness, s3

s3=1/ 3/2

( ttm )3 E ( t ) dt
0

=
1
1.1854 3/ 2

6.00

[0+ 4 ( 0 )+ 2 ( 0 )+ 4 ( 0 )+2 (0.9710 ) +4 (0.9805 )+2 (0.3458 ) +4 (0.0604 ) +2 (0.0006 )+

0.5
3
0

1/ 3/2

( ttm )3 E ( t ) dt=0.4096
0

min3

8) DISCUSSION

Firstly, the objectives 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 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.
For this experiment, we examine 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 these types of 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
2.1 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 shows that the result did not differ from the theory that recorded that the
conductivity is reaching zero at time of 4 minutes. Thus, experiment 1 is a succeess.
16

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 3.1 mS/min and
then undergoes some increment until at minute 6.0 which the outlet conductivity is 2.0
mS/min.
The construction of the residence time distribution (RTD) function for the tubular
flow reactor for pulse input and also step change is done after that. 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 is almost same with the graph that is stated
at the theory. From the graph, it can be concluded that the residence time distribution is
depends on the outlet conductivity.
The other 3 data that had been obtained and calculated are mean residence time, t m
variance (second moment), 2 and skewness (third moment), s3 that recorded 1.0000,
0.7361 and 1.1776 respectively. The skewness for the pulse input give a positive value and
it called positive skew.
Compared of the step change, the graph is 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 4.1334 minutes.
The other 2 data that are calculated which are variance (second moment), 2 and skewness
(third moment), s3 are 1.4051 and -0.4096 respectively. The skewness gives a negative
value and it is called negative skew compare to pulse input.

9) CONCLUSION
For both experiment, all objectives are achieved successfully. For the first experiment, the
effect of a pulse input is examined and a RTD for tubular flow is constructed. Same goes
for experiment two where the effect of a step change input in tubular flow reactor is
recognised and a RTD was also constructed.

10) RECOMMENDATION
17

Each experiment must perform general start-up and shut-down procedure to make

sure the experiment runs smoothly.

Open and close the valve carefully according to the procedure given.
Make sure there is no leakage at the equipment.
Flow rate of the reactant must remain constant throughout the experiment.
Make sure the inlet and outlet conductivity are stable before starting the
experiment.

11) REFERENCE

Levenspiel, Octave (1999). Chemical Reaction Engineering (3rd ed.). John Wiley

& Sons.
Nauman, E. Bruce (2004). "Residence Time Distributions". Handbook of Industrial

Mixing: Science and Practice. Wiley Interscience. pp. 117.

Tubular Flow Reactor Static Mixer. (n.d.). Retrieved April 29, 2015, from

http://www.stamixco-usa.com/tubular-flow-reactors
(K. G. Denbigh, Chemical Reactor Theory: An Introduction, 41-45)

18

12) APPENDIX

19