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 dependant variables are
functions of position within the reactor rather than of time. This experiment is conducted to
achieve 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
3 1
experiment, the flow rate was set up at 700 m s
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
Q 2 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
function 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 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 stimulusresponse 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.

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.

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 backmixing 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.
3

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

t = 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

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.

APPARATUS AND MATERIAL

Tubular flow reactor

Deionized water
Sodium chloride solution (NaCl)

Plug Flow Reactor

PROCEDURE
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.

Experimental procedure
a) Experiment 1: Pulse Input in a Tubular Flow Reactor
1. The general start-up procedure was performed as stated above.
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.

b) 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.

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.

RESULT
Experiment 1: Pulse Input in a Tubular Flow Reactor
Flow rate = 700 mL/min
Input Type = Pulse input
Time (min)

Conductivity (mS/cm)

Inlet

Outlet

0.0

0.33

0.50

0.5

0.33

0.50

1.0

0.00

3.10

1.5

0.00

3.10

2.0

0.00

3.20

2.5

0.00

1.80

3.0

0.00

0.40

3.5

0.00

0.10

4.0

0.00

0.00

Outlet conductivity vs Time

3.5

3.1

3.1

3.2

3
2.5
1.8

Conductivity (mS/cm)

1.5
1
0.5
0.5

0.5

0.4
0.1

3.5

0
0

0.5

1.5

2.5

4.5

Time (min)
GRAPH 1 : OUTLET CONDUCTVITY VS TIME

10

Sample Calculation

in
For time 0.0 to 0.5 minutes
1
Area= (0.50+0.50)(0.50.0)
2
= 0.25
Time
(min)

Conductivity (mS/cm)

Inlet

Outlet

0.33
0.33
0.0
0.0
0.0
0.0
0.0
0.0
0.0

0.50
0.50
3.10
3.10
3.20
1.80
0.40
0.10
0.00

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0

E(t)

0.25
0.375
1.55
1.575
1.25
1.60
0.125
0.025
0.00

0.0741
0.0741
0.4593
0.4593
0.4741
0.2667
0.0593
0.0148
0.000

So the total area of

= (0.25+0.375+1.55+1.575+1.25+1.60+0.125+0.025) = 6.75

11

Chart Title
0.5
0.45
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0

0.5

1.5

2.5

3.5

Column2

GRAPH 2 : E(t) VS TIME

For time 0.0 to 0.5 minutes

1
Area= (0.0741+0.0741)( 0.5)
2

=0.03705

So the total area of

(0.03705+0.13335+0.22965+0.23335+0.1852+0.0815+0.018525+0.0037+0.0000) = 0.9223

12

Residence time,

4(0.9223) = 3.6893

Time (min)

E(t)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0

0.0741
0.0741
0.4593
0.4593
0.4741
0.2667
0.0593
0.0148
0.000

= 3.03044

0.000
0.03705
0.4593
0.6894
0.9482
0.66679
0.1779
0.0518
0.000

0
0.753718
3.321811
2.201441
1.352955
0.377229
0.028916
0.000530

0
-2.403833
-8.933347
-4.819614
-2.285548
-0.448639
-0.019421
-0.000395

0.000

0.000

= 8.0366

Mean residence time,

= -18.9108

3.03044

Second moment, Variance,

= 8.0366

Third moment, Skewness, s3=

1
=

( 8.0366 )

3
2

(18.9109 ) =0.83004

13

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
0
0
2.5
0
2.7
0
2.8
0
2.8
0.1
2.8
1.4
2.9
1.8
2.9
2.1
2.9
2.3
2.9
2.4
2.9
2.6

Outlet conductivity vs Time

3
2.5
2

Outlet Conductivity (mS/cm)

1.5

Column3

1
0.5
0

0.5

1.5

2.5

3.5

4.5

Time(min)

Graph of Outlet Conductivity vs Time

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Time
(min)

Conductivity
(mS/cm)
Inlet
Inlet

C(t)

E(t)

Ci t

Ci t

Ci t
0.0
0.5
1.0
1.5
2.0

0
2.5
2.7
2.8
2.8

0
0
0
0
0.1

2.5

2.9

1.4

3.0

2.9

1.8

3.5

2.9

2.1

0
0
0
0

13

0
0
0
0
0.00404
4
0.07077
9
0.10920
1
0.14863
5
0.18604
7
0.21840
2
0.26289
2

49.45

0.2
3.5
5.4
7.35
4.0

2.9

2.3
9.2

4.5

2.9

2.4

5.0

2.9

2.6

10.8

Total

tm

tE (t)
Ci t

( tt m ) E(t )

( tt m ) E(t )

Ci t

Ci t

0
0
0
0
0.00016
4
0.00357
8
6.63E03
0.01052
0
0.01504
9
0.01987
5
0.02658
2
0.08239
8

s3
3

0
0
0
0

0
0
0
0

0.000327

0.000654

0.00892

0.022268

0.019787

0.059230

0.036600

0.127714

0.059745

0.238081

0.088648

0.397156

0.131499

0.653997

0.345526

1.4991

Residence time distribution (RTD) function plug flow reactor

E(t)
0.3
0.25
0.2
E(t)
0.15
0.1
0.05
0
0

0.5

1.5

2.5

3.5

4.5

15

16

Sample of Calculation

C (t )
0

dt =

Ci t

= Area

So based on the Table, Area is 49.45 m

Example of calculation at t =2.50 min
tm =

t E(t )
Area

tm =

2.50 0.070778
49.45

t m = 0.003578

2
( tt m ) E (t)

Area

( 2.500.003578 )2 0.070778
49.45

2 = 0.00892

s3 =

( t t m ) E(t )
Area

( 2.500.003578 )3 0.070778
49.45

s 3 = 0.022268

17

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 3.2 mS/cm at
time of 2 minutes which are the highest value. After that, the conductivity is decrease within
the time and finally at time 4 minutes the conductivity 0 mS/cm. From the result, it shows
that the result did not differ from the theory. Thus, experiment 1 is a succeess.
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 is the inlet conductivity is 2.8 mS/cm and then
undergoes some increment until at minute 5.0 which the outlet conductivity is 2.6 mS/cm.
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.

18

The other 3 data that had been obtained and calculated are mean residence time, tm
variance (second moment), 2 and skewness (third moment), s3 that recorded 3.03044,
8.0366 and -0.83004 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, t m is 0.082398. The other 2 data that are calculated
which are variance (second moment), 2 and skewness (third moment), s3 are 0.345526 and
1.4991 respectively. The skewness gives a negative value and it is called negative skew
compare to pulse input.

19

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.

RECOMMENDATION

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.

20

REFERENCES

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)

21

APPENDICES
Tubular Flow Reactor : SOLTEQ Model : BP 101

22

23