TABLE OF CONTENT

NO

TITLE

PAGES

1.0

Abstract

2.0

Introduction

3-6

3.0

Objectives

5.0

Apparatus

6.0

Experimental procedure

7-8

7.0

Results & calculation

8.0

Discussion

9.0

Conclusion

10.0

Recommendations

11.0

References

12.0

Appendices

10

ABSTRACT

This experiment is conducted to achieve the objectives that has been

considered which is to examine the effect of pulse input in a tubular flow
reactor, to construct a residence time distribution (RTD) function for the
tubular flow reactor, and to examine the effect of step change input in a
tubular flow reactor. The experiment is divided into two that is 1) pulse input
in a tubular flow reactor; and 2) step change input in a tubular flow reactor.
The C(t) calculated for pulse and step change input are 5.30 and 8.30
respectively. As for pulse input, the mean residence time, variance, skewness
calculate is 0.2465min, 0.3753min, and 0.6992min respectively. Meanwhile,
the mean residence time, variance, skewness calculated for step change
input is 0.4354min, 1.6245min, and 6.5121min respectively. The residence
time distribution, RTD function is plotted for both pulse and step change
input and it show that the function is dependent with the outlet conductivity
of the system.

INTRODUCTION
Tubular flow reactor (TFR) is any continuously operating reactor in which
there is a steady movement of one or all of the reagents in a chosen spatial
direction (enter at one end of the system and leaving the other) and in which
no attempt is made to induce mixing between elements of fluid at different
points along the direction of flow (K. G. Denbigh, 1984).
The type of flow in TFR can be laminar, as with viscous fluids in small
diameter tube and greatly deviate from ideal plug flow behavior, or
turbulent, as with gases. TFR generally preferred to laminar flow due to the
mixing and heat transfers are improved. Establishing turbulent flow for slow
reactions and especially in small laboratory and pilot-plant reactors can leads
to inconveniently long reactors or may require unacceptably high feed rates
TFR are also used for catalytic reactions. The reactor here is often
referred to as a fixed-bed reactor as it is packed with particles of the solid
catalyst. The reactor may be one large-diameter cylinder, or it may consist of
many tubes in parallel, fixed between two header as in a tube-and-shell heat
exchanger. Parts that need to be extra cautions with when designing any
type of reactors are the performance of the reactor when running steadily,
the means of arriving at that state and stopping the process, either for
routine maintenance or in the case of breakdown and not to forget the
conditions of the area of the reactor to be build.
The diameter of a cylindrical TFR should clearly be small, in order to
decrease the distance over which the heat must be conducted up to the wall.
It may be necessary to immerse cooling coils in the body of the catalyst
when there are compelling reasons of a different kind for choosing a large
diameter, or for placing the catalyst in large trays.
These tubular reactors are used in varieties of industries (Parr
Instrument Company, 2015):

Petroleum
Petrochemical
Polymer
Pharmaceutical
Waste Treatment
Specialty Chemical
Alternative Energy

It is also are used in a variety of applications:

Carbonylation
Dehydrogenation
Hydrogenation
Hydrocracking
Hydroformulation
Oxidative Decomposition
Partial Oxidation
Polymerization
Reforming

The non-ideality of industrial and natural processes leads engineers to

develop corrections to the ideal models, in order to use them with less restriction.
For this reason, it is defined a residence time distribution, which is a function that
describes the evolution of the average instantaneous concentration versus the
elapsed time (Stenstrom, 2003). It is very convenient to express the residence time
distribution as the normalized function E,

E (t)=

c(t )

c ( t ) . dt
0

FIGURE
RTD is used to characterize the mixing and flow within reactors and to
compare the behavior of real reactors to their ideal model. This is very useful
as not only for troubleshooting existing reactors, but in estimating the yield
of a given reaction and designing future reactors. It generally begins with
three assumptions:
1. The reactor is at steady state;
2. Transports at the inlet and the outlet takes place only by advection (a
transport mechanism of a substance by a fluid due to the fluids bulk
motion); and
3. The flow is incompressible.
Residence time distributions are measured by introducing a non-relative
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 or change the physical characteristics of the fluid and the
introduction of the tracer itself should not modify the hydronamic conditions.
Generally, the change occur in tracer will either be a pulse or a step.
As for pulse experiments, it requires the introduction of a very small
volume of concentrated tracer at the inlet of the reactor. If a mass of tracer,
M, is introduced into a vessel of volume V, and an expected residence time

of

, the resulting curve of C (t) can be transformed into a dimensionless

residence time distribution curve by following equation :

E (t)=

c(t )

c ( t ) . dt
0

The concentration of tracer at the reactor inlet changes abruptly from

0 to C0 in a step change experiment. The concentration of tracer at the
outlet is measured and normalized to concentration C0 to obtain the nondimensionless curve F(t) which goes from 0 to 1:
F ( t )=

c (t )
c0

OBJECTIVE(S)
Experiment 1
1. To examine the effect of pulse input in a tubular flow reactor.
2. To construct a residence time distribution (RTD) function for the tubular
flow reactor.
Experiment 2
1. To examine the effect of step change input in a tubular flow reactor.
2. To construct a residence time distribution (RTD) function for the tubular
flow reactor.

MATERIALS & APPARATUS

Tubular Flow Reactor

Deionized Water

X
X

PROCEDURES
Experiment 1: Pulse input in a tubular flow reactor
1. General start-up procedures are performed.
2. Valve V9 is opened and then pump is switch on.
3. Pump 1 flow controller is adjusted to give a constant flow rate of deionized water into the reactor R1 at approximately 700mL/min at FI-01.
4. The de-ionized water is let alone 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 are recorded.
5. Valve V9 is closed and pump P1 is switched off.
6. Then, valve 11 is opened and pump 2 is switched on. The timer is
started simultaneously.
7. Pump 2 flow controller is adjusted to give a constant flow rate of salt
solution into the reactor R1 at 700mL/min at FI-02.
8. The salt solution is left to flow for 1 minute, and then the timer is reset
and starts again. This will start the time at the average pulse input.
9. Valve 11 is closed and pump 2 is switched off. Then, valve V9 is quickly
opened and switched on pump 1.
10.
The de-ionized water flow rate is ensured to be maintained at
700mL/min by adjusting P1 flow controller.
11.
Both the inlet (QI-01) and outlet (QI-02) conductivity values are
recorded at regular intervals of 30 seconds.
12.
The conductivity values are continued to be recorded until all
reading are almost constant and approached the stable low level
values.
Experiment 2: Step change input in a tubular flow reactor
1. The general start up procedures is performed.

2. Valve V9 is opened and pump P1 is switched on.

3. Pump P1 flow rate controller is adjusted to give a constant flow rate of
de-ionized water into the reactor R1 at approximately 700mL/min at FI01.
4. The de-ionized water if left 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 are then recorded.
5. Valve V9 is closed and pump P1 is switched off.
6. Then, valve 11 is opened and pump 2 is switched on. The timer is
started simultaneously.
7. Both the inlet (QI-01) and outlet (QI-02) conductivity values are
recorded at regular intervals of 30 seconds.
8. The conductivity values are continued to be recorded until all reading
are almost constant.

DIAGRAM(S)

RESULT(S)
Experiment 1: Pulse input in a tubular flow reactor
Flow rate : 700 mL/min
Input type : Pulse input
tm

s3

(mean

(second

(third

(mi

residence

moment,

moment,

n)

time)

variance

skewnes

Tim

Conductivit

y (mS/cm)

Inlet

Outle

C(t)

Cit

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

0.2
0.2
0.1
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0

2.6
2.6
2.6
2.7
2.0
0.5
0.1
0.1
0.0
0.0
0.0

0.00
1.30
1.30
1.35
1.00
0.25
0.05
0.05
0.00
0.00
0.00
=5.3
0

E(t)

Cit /

t * E(t) /

(t-tm) *

s)
(t-tm)3 *

Cit

Cit

E(t) /

E(t) /

0.0000
0.0231
0.0463
0.0721
0.0712
0.0223
0.0053
0.0062
0.0000
0.0000
0.0000
=0.2465

Cit
0.0000
0.0105
0.0421
0.0980
0.1325
0.0547
0.0159
0.0216
0.000
0.000
0.000
=0.3753

Cit
0.0000
0.0050
0.0401
0.1399
0.2555
0.1355
0.0476
0.0756
0.0000
0.0000
0.0000
=0.6992

0.0000
0.2453
0.2453
0.2547
0.1887
0.0472
0.0094
0.0094
0.000
0.000
0.000
=1.000
0
TABLE

Conductivity (outlet) vs Time

3
2.5
2
Outlet Conductivity (ms/cm)

1.5
1
0.5
0

0.5

1.5

2.5

3.5

4.5

4.5

Time (min)

FIGURE

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

0.15
0.1
0.05
0

0.5

1.5

2.5

Time (min)

FIGURE

3.5

Experiment 2: Step change input in a tubular flow reactor

Flow rate : 700 mL/min
Input type : tubular
tm

s3

(mean

(second

(third

(mi

residence

moment,

moment,

n)

time)

variance

skewnes

Tim

Conductivit

y (ms/cm)

Inlet

Outle

C(t)

Cit

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

0.0
3.6
3.7
3.8
3.8
3.9
3.9
3.9
3.9
3.9
3.9

0.0
0.0
0.0
0.0
1.6
2.3
2.4
2.5
2.6
2.6
2.6

0.00
0.00
0.00
0.00
0.80
1.15
1.20
1.25
1.30
1.30
1.30
=8.3
0

E(t)

Cit /

t * E(t) /

(t-tm) *

s)
(t-tm)3 *

Cit

Cit

E(t) /

E(t) /

0.0000
0.0000
0.0000
0.0000
0.0232
0.0417
0.0523
0.0635
0.0755
0.0849
0.0943
=0.4354

Cit
0.0000
0.0000
0.0000
0.0000
0.0454
0.1009
0.1514
0.2143
0.2906
0.3678
0.4541
=1.6245

Cit
0.0000
0.0000
0.0000
0.0000
0.0897
0.2481
0.4462
0.7364
1.1404
1.6238
2.2275
=6.5121

0.0000
0.0000
0.0000
0.0000
0.0964
0.1386
0.1446
0.1506
0.1566
0.1566
0.1566
=1.000
0
TABLE

Conductivity (outlet) vs Time

3
2.5
2
Outlet Conductivity (ms/cm)

1.5
1
0.5
0

0.5

1.5

2.5

3.5

4.5

Time (min)

FIGURE

E(t) vs Time
0.18
0.16
0.14
0.12
0.1
E(t)

0.08
0.06
0.04
0.02
0

0.5

1.5

2.5

Time (min)

FIGURE

3.5

4.5

SAMPLE OF CALCULATION(S)
Experiment 2
Area, C(t) = Cit ; where Ci is the outlet conductivity and t = 0.5
At t = 3.0 min
C(t) = 2.4(0.5) = 1.20
E(t) = Cit / Cit
At t = 3.0 min
E(t) = 1.20/8.30 = 0.1446
Mean Residence Time, tm = t x E(t) / Cit
At t = 3.0 min
tm = 3.0(0.1446) / 8.30 = 0.0523
Variance, 2 = (t-tm)2 x E(t) / Cit
At t = 3.0 min
2 = (3.0 0.0523)2 x 0.1446 / 8.3 = 0.1514
Skewdness, s3 = (t-tm)3 x E(t) / Cit
At t = 3.0 min
s3 = (3 0.0523)3 x 0.1446 / 8.3 = 0.4462

*calculations for Experiment 1 is as the same as Experiment 2

DISCUSSION
The objectives needed to be achieved in this experiment are to determine
the effect of pulse and step change in tubular flow reactor and also to
construct the RTD function for this reactor at the end of the experiment. The
flow rate of de-ionized water is set constant at 700mL/min. the conductivity
for the inlet and outlet of the solution had been recorded at the period of
time until the conductivity of the solution is constant.
As for pulse input, the data collected were tabulated and graph of
outlet conductivity versus time was plotted to obtain a C(t) curve. At minute
of 1.5, the conductivity recorded is 2.7 mS/cm which was the highest value
for the outlet solution. Then, the slope of the graph seems to be decreasing
within the time and come to a constant value, 0 mS/cm at minute of 4. From
the results obtained, it was not differ from theory that state the conductivity
is reaching zero at time of 4 minutes. Thus, experiment 1 is considered
succeed.
As for step change input, graph of outlet conductivity against time was
also plotted from the data obtained from the experiment conducted. The
slope of the graph started to increase at 2 minutes with the value outlet
conductivity of 1.6 mS/cm. there are difference between both of pulse and
step change input graph that is for the pulse, the slope was decreasing and
meanwhile the step change slope was increasing within time before coming
into a constant value of outlet conductivity.
Residence time distribution function was constructed after calculated
the information needed and it has been tabulated in the results part. The
graph was plotted based on exit time E(t) versus time. The RTD calculated
for pulse input using equation Cit / Cit was 1. Besides that, there are 3
other factors that were calculated, that is mean residence time, variance,
and skewness and the value for each are 0.246min, 0.3753min, and
0.6992min respectively.

As for step change input, the RTD function obtained also shows that it
depends on the outlet conductivity of the solution as the slope are the same;
increasing with time before arriving at constant value. The value calculated
for mean residence time, variance, and skewness are 0.4354min, 1.6245min,
and 6.5121min respectively.

CONCLUSION
The experiment conducted is considered as a success as the objectives are
achieved, that is to examine the effect of a pulse and step change input in a
tubular flow reactor and to construct a residence time distribution (RTD)
function for the tubular flow reactor. Even though the data collected are not
very accurate due to certain errors occurred during conducting the
experiments, graphs of residence time distribution is able to be plotted and
the errors presence has been discussed in the discussion part.
The distribution of exit time E(t) is calculated for each 30 seconds until
5 minutes interval. The sum of E(t) for pulse and step change input is 1. The
mean residence time for pulse input is 0.2465 minutes and for step change
input is 0.4354 minute.
The variance and skewness are also calculated. As for pulse input, the
value is 0.3753 minute and 0.6992 minute respectively, while for step
change is 1.6245 minutes and 6.5121 minutes. Graphs of C(t) against time
and distribution of exit time E(t) versus time are plotted, and the slope
obtained shows that E(t) does depends on the value of C(t).

RECOMMENDATION(S)
In order to improvise the results obtained, there are certain recommendation
such as the reactor is ensured no leakages before doing the start-up
procedures. Besides that, the general start-up and shut-down must be

conducted to make sure there is no left over in the chamber after an

experiment has been conducted. Another recommendation is that the valves
and the pump should be opened or closed and switch on or off carefully
according to the steps stated in the procedures.

REFERRENCES
1. K. G. Denbigh, J. C. (1984). Chemical Reactor Theory: An Introduction.
Cambridge University Press.
2. Parr Instrument Company. (2015). About Us: Parr Instrument Company.
Retrieved

from

5400

Continuous

Flow

Tubular

Reactors:

http://www.parrinst.com
3. Stenstrom, M. K. (2003). Fundamentals of Chemical Reactor Theory.
Los Angeles: University of California, Los Angeles.
4. Turbular

FLow

Reactor.

(n.d.).

Retrieved

April

2013,

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

from

APPENDICES