ABSTRACT

From this experiment, our objectives are to examine the effect of pulse input and step change
in a tubular flow reactor and to construct a residence time distribution (RTD) function for the
tubular flow reactor. In the pulse input experiment, the flow rate was set up at 700 mL/min
and let it for one minute before the valve is open and the reading taken every 30 seconds until
the conductivity reading is 0.0. In the other hand, the step change experiment, the
conductivity were observe every 30 seconds until the reading at outlet conductivity is
constant for 3 times in which in this experiment the constant value was 2.6. For the first
experiment, the final conductivity for inlet and outlet are 0.0 mS/cm and 0.0 mS/cm while for
the second experiment are 3.9 mS/cm and 2.6 mS/cm. The outlet conductivity, C(t) is
calculated and we get 5.3 for the first experiment and 8.3 for the second experiment. Then,
we are able to determine the distribution of exit time, E(t) for each 30 seconds. The sum of
E(t) we get is 1.0000 for both experiment which is the residence time distribution for the
experiment. The total mean residence time, tm for both experiment are 0.2465 minute and
0.4354 minutes respectively. The sum of variance, 2 and the skewness, s3 are also then
calculated. The value we get for both experiment for 2 is 0.3665 and 1.6245, for the s3 is
0.6992 and 6.5121 respectively. Graphs for outlet conductivity, C(t) against time and
distribution of exit time, E(t) against time is plotted. The plotted graph shows that the value
of E(t) is depends on the value of C(t) in which is the same concept with the theory.

TABLE OF CONTENT
PAGE
ABSTRACT

TABLE OF CONTENT

INTRODUCTION

OBJECTIVE

THEORY

APPARATUS

PROCEDURE

RESULTS

SAMPLE OF CALCULATION

12

DISCUSSION

13

CONCLUSION

14

RECOMMENDATION

14

REFERENCES

15

APPENDIXES

16

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. 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. Flow in tubular reactor can be laminar or turbulent. Turbulent flow generally is
preferred to laminar flow, because mixing and heat transfer are improved.
The reactants are continually consumed as they flow down the length of the reactor in
the tubular reactor. However, many tubular reactors that are used to carry out a reaction do
not fully conform to this idealized flow concept. 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.
For most chemical reactions, it is impossible for the reaction to proceed to 100%
completion. The rate of reaction decreases as the per cent completion increases until the point
where the system reaches dynamic equilibrium (no net reaction, or change in chemical
species occurs). The equilibrium point for most systems is less than 100% complete. For this
reason a separation process, such as distillation, often follows a chemical reactor in order to
separate any remaining reagents or by products from the desired product. These reagents may
sometimes be reused at the beginning of the process, such as in the Haber process.
High temperature reactions Residence Time Distribution (RTD) analysis is a very
efficient diagnosis tool that can be used to inspect the malfunction of chemical reactors. It can
also be very useful in the estimation of effluent properties and in modelling reactor behaviour.
This technique is extremely important in teaching reaction engineering, in particular when the
non-ideal reactors become the issue. Residence time distributions are measured by
introducing an impulse and step tracer technique into the system. The concentration of the
tracer is changed according to a known function and the response is found by measuring the
3

concentration of the tracer at the outlet. The RTD technique has also been used for the
experimental characterization of flow pattern of a packed bed and a tubular reactor that
exhibit, respectively, axially dispersed plug flow and laminar flow patterns.
Another important field of RTD applications lies in the prediction of the real reactor
performance. Nowadays, the concepts of macro and micro mixing are fundamental. Each
macro mixing level is expressed in the form of a specific RTD. There is a given micro mixing
level, which lies between two limiting cases, complete segregation and perfect micro mixing.

OBJECTIVE

1) To examine the effect of pulse input in tubular flow reactor.

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

THEORY

Tubular reactors are 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.
In a tubular flow reactor, the feed enters at one end of a cylindrical tube and the
product stream leaves at the other end. The long tube and the lack of provision for stirring
prevent complete mixing of the fluid in the tube. Hence the properties of the flowing stream
will vary from one point to another, namely in both radial and axial directions. It is often not
necessary to know details of the entire flow fluid but rather only how long fluid elements
reside in the reactor (i.e. the distribution of residence times). This information can be used as
a diagnostic tool to ascertain flow characteristics of a particular reactor.

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.
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.
In order to analyse the residence time distribution of the fluid in a reactor the
following relationships have been developed. Fluid elements may require differing lengths of
time to travel through the reactor. The distribution of the exit times, defined as the E(t) curve,
is the RTD of the fluid. The outlet conductivity of a tracer species C(t) can be used to define
E(t). That is:
E (t)

Ctout (t )

C tout ( t ) dt
0

Based on the data collected, a graph of conductivity versus time could be draw to
obtain the C(t) curve and data of the integral C(t) could be calculate.

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

If the RTD function, E(t), is very broad, however, it may be difficult to inject an
amount of tracer that is sufficiently large so as to keep the outlet concentration sufficiently
high to be measured accurately.

APPARATUS
1) Soltec Tubular Flow Reactor instrument
2) Clock watch
3) Solution 0.025M Sodium Chloride and De-ionized water.

PROCEDURE
Experiment 1:
1. Perform the general start-up procedure as the manual instructed.
2. Valve V9 is opened and pump P1 is switched on.
3. The P1 pump is adjusted by controlling the flow controller to obtain a flow rate of
approximately 700mL/min at Fl-01 of de-ionized water into the reactor R1.
4. The de-ionized water is allowed to continue flowing through the reactor until the inlet
(Q1-01) and outlet (Q1-02) conductivity values are stable at low levels. Both
conductivity values are recorded.
5. Valve V9 is closed and pump P1 is switched off.
6. Valve V11 is opened and pump P2 is switched on. The timer is simultaneously started.
7. Pump P2 flow controller is adjusted to give a constant flow rate of salt solution into
the reactor R1 at 700mL/min at F1-02.
8. The salt solution is allowed to flow for 1 minute, the timer is reset and restarted. This
will start the time at the average pulse input.
9. Valve V11 is closed and pump P2 is switched off. Valve V9 is quickly opened and
pump P1 is switch on.
10. By adjusting pump P1 flow controller, the de-ionized water flow rate is always
maintained at 700mL/min.
11. The inlet (Q1-01) and outlet (Q1-02) conductivity values are recorded at regular
interval of 30 seconds.
12. The conductivity values are recorded until all readings are almost constant and
approach stable low level values.

Experiment 2:
1. Closed all the pump and valve from the experiment 1.
2. Valve V9 is opened and pump P1 is switched on.
3. The P1 pump is adjusted by controlling the flow controller to obtain a flow rate of
approximately 700mL/min at Fl-01 of de-ionized water into the reactor R1.

4. The de-ionized water is allowed to continue flowing through the reactor until the inlet
(Q1-01) and outlet (Q1-02) conductivity values are stable at low levels. Both
conductivity values are recorded.
5. Valve V9 is closed and pump P1 is switched off.
6. Valve V11 is opened and pump P2 is switched on. The timer is simultaneously started.
7. The inlet (Q1-01) and outlet (Q1-02) conductivity values are recorded at regular
interval of 30 seconds.
8. The conductivity values are recorded until all readings are almost constant.
RESULTS
Experiment 1: Pulse input in a Tubular Flow Reactor
Flow rate

= 700 mL/min

Input type

= Pulse input

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 (Co)
Outlet (Ci)
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

Outlet Conductivity vs Time

3
2.5
2
Outlet Conductivity (mS/cm)

1.5
1
0.5
0
0

Time (min)

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

C(t)

E(t)

Outlet (Ci)

Cit

Ci(t)

0.0000
1.3000
1.3000
1.3500
1.0000
0.2500
0.0500
0.0500
0.0000
0.0000
0.0000

Ci(t)
0.0000
0.2453
0.2453
0.2547
0.1887
0.0472
0.0094
0.0094
0.0000
0.0000
0.0000

2.6
2.6
2.6
2.7
2.0
0.5
0.1
0.1
0.0
0.0
0.0

Residence time distribution (RTD) function for tubular flow reactor

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

0.15
0.1
0.05
0
0

Time (min)

Time (min)

Outlet

E(t)

tm= tE(t)

(Ci)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

2.6
2.6
2.6
2.7
2.0
0.5
0.1
0.1
0.0
0.0
0.0
Total () =

0.0000
0.2453
0.2453
0.2547
0.1887
0.0472
0.0094
0.0094
0.0000
0.0000
0.0000
1.0000

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

2 =

S3 =

(t - tm)2*

(t - tm)3*

E(t)/

E(t)/

C i t

C i t

0.0000
0.0105
0.0421
0.0980
0.1325
0.0547
0.0071
0.0216
0.0000
0.0000
0.0000
0.3665

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

Experiment 2: Step change input in a Tubular Flow Reactor

Flow rate

= 700 mL/min

Input type

= Step change
9

Conductivity (ms/cm)
Inlet (Co)
Outlet (Ci)

Time (min)
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

Outlet conductivity vs Time

3
2.5
2
Oulet Cnductivity (mS/cm)

1.5
1
0.5
0
0

Time (min)

Time
(min)

0.0
0.5
1.0
1.5

Conductivity (mS/cm)
Inlet
Outlet
(Co)

(Ci)

0.0
3.6
3.7
3.8

0.0
0.0
0.0
0.0

C(t)
Cit

E(t)
Ci(t)
Ci(t)

0.0000
0.0000
0.0000
0.0000

0.0000
0.0000
0.0000
0.0000

tm
2
t*E(t)/
(t - tm) 2 *
C i t
E(t)/
C i t
0.0000
0.0000
0.0000
0.0000

0.0000
0.0000
0.0000
0.0000

S3
(t - tm) 3 *
E(t)/
C i t
0.0000
0.0000
0.0000
0.0000
10

2.0
2.5
3.0
3.5
4.0
4.5
5.0

3.8
3.9
3.9
3.9
3.9
3.9
3.9

1.6
2.3
2.4
2.5
2.6
2.6
2.6
Total () =

0.8000
1.1500
1.2000
1.2500
1.3000
1.3000
1.3000
8.3000

0.0964
0.1386
0.1446
0.1506
0.1566
0.1566
0.1566
1.0000

0.0232
0.0417
0.0523
0.0635
0.0755
0.0849
0.0943
0.4354

0.0454
0.1009
0.1514
0.2143
0.2906
0.3678
0.4541
1.6245

0.0897
0.2481
0.4462
0.7364
1.1404
1.6238
2.2275
6.5121

Residence time distribution (RTD) function for tubular flow reactor

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

Time (min)

SAMPLE OF CALCULATION

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

Area = (0.0X0.0)+(0.0X0.5) +(0.0X0.5)+(0.0X0.5)+(1.6X0.5)+ (2.3X0.5)+(2.4X0.5)

+(2.5X0.5)+(2.6X0.5) +(2.6X0.5) +(2.6X0.5).
Area = 8.3000
11

t m=

t E( t)
Area

t m=

2.0 0.0964
8.3000

t m=0.0232

2=

2
( tt m ) E(t)

Area

( 2.00.0232 )2 0.0964
8.3000

2=0.0454

s=

s 3=

3
( t t m ) E(t )

Area

( 2.00.0232 )3 0.0964
8.3000

s =0.0897

DISCUSSION

12

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. De-ionized water and Salts solution was used as chemicals to determine the
conductivity. The experiment was run at flow rate of 700mL/min. The conductivity for the
inlet and outlet was recorded from time equal to t0=0 until them both reaching a constant
value for itself.
For 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 2.6 mS/cm
during the experiment started which is 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 the results was not differ from the theory that recorded that the conductivity is
reaching zero at time of 4 minutes. Thus, the experiment 1 is succeeded. However, some of
the unexpected error may occur during the experiment because the outlet conductivity should
starts lower and increase and decrease again so that we can calculate the area under the graph
more accurate.
In addition, for the graph of step change the outlet conductivity is increases within the
time by started at time of 2.0 minutes which it inlet conductivity is 3.8 mS/cm and then
increase until at minutes 3.5 and then the value of the outlet conductivity is constant at 2.6
mS/cm till minutes 5.
To construct a residence time distribution (RTD) function for the tubular flow reactor
with pulse input and step change, the graph based on exit time (E(t)) versus time were
plotted. Both the RTD and outlet conductivity versus time graph were almost the same for
both input. From the graph, it can be concluded that the residence time distribution is depends
on the outlet conductivity.

CONCLUSION

13

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. For
experiment 1, the effect of pulse input in a tubular flow reactor was examined. The flow rate
was kept constant at 700 ml/min. The summation of C(t) is 5.3, and the sum of E(t) came to a
result of 1.0000. As seen from the graph, both outlet conductivity and E(t) remained constant
until minute 1.5, then took a sharp decrease until minute 3, and then the outlet conductivity is
constant 0 mS/cm till minutes 5. For experiment 2, the effect of a step change input was
examined. The flow rate was also kept constant at 700 ml/min. The results and calculations
shows that the summation of the conductivity was 8.3000 and the sum of E(t) was 1.0000.
From the both graphs plotted, it is seen that the data is constant till minute 1.5 and then
increases sharply until minute 4 after that, the graph is constant. The experiment was
considered a success as all objectives were achieved.

RECOMMENDATION
There are several recommendations that can be taken in order to get more accurate result or
lower the percentage error that are:
1) Make sure that certain valve need to be open and closed rapidly, so one person must
handle this valve with efficiently to get more accurate reading.
2) The flow rate of fluid in the reactor must constant all the time during the experiment.
This is because the flow rate is always reset when we switch on and off the pump.
3) To obtain more understanding about this experiment, its recommend to use another
solvent and solute.

REFERENCES

14

Jorge A.T.A.D., Paula R.P., Jorge A.W.G., (2013). Determination of the effective radial mass
diffusivity in tubular reactors under non-Newtonian laminar flow using residence time
distribution data. International Journal of Heat and Mass Transfer. Vol. 71. 18-25.
National Technical University of Athens (NTUA). (n.d.). Tubular reactor or plug flow reactor.
http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm.
Reactor pilot plant manual laboratories provided by instructor.
Kanse N.G., Dawande S.D. (2012). RTD Studies in Plug Flow Reactor and its Simulation
with Comparing Non Ideal Reactors. Research Journal of Recent Sciences Vol. 1(2),
42-48.
http://caltechbook.library.caltech.edu/274/9/FundChemReaxEngCh8.pdf

APPENDIXES

15

Figure 1: Soltec Tubular Flow Reactor instrument

16