ABSTRACT

Two experiments were conducted for tubular flow reactor (TFR). The objectives for
the first experiment is to examine the effect of a pulse input in tubular flow reactor and to
construct a residence time distribution (RTD) function for the tubular reactor. The second
objective for experiment 2 is to examine the effect of a step change input in tubular flow
reactor and to construct a residence time distribution (RTD) function for the tubular flow
reactor. The experiment is start first by taking the inlet and outlet conductivity. Then, the
graph is plot and the C(t) is obtained before the E(t) curve can be plotted. From the E(t)
curve, the area under graph is obtained. Based on that, calculation have been made to get the
readings for mean residence time, second moment or variance and third moment or also
known as skewness. From the graph of first experiment, it showed that the residence time
distribution (RTD) for pulse input increased with time. After a few minutes, it will slowly
decreases until the value of zero. While for the second experiment, it can be seen that the
value slowly increase of outlet conductivity and E(t), the outlet conductivity reached constant
at last. The mean residence time, second moment (Variance) and third moment (Skewness)
were calculated was calculated from the graph. For the first experiment, the value of mean
residence time is 1.4667 min, the second moment (Variance) is 0.4756 min2 and the third
moment (Skewness) is 0.3746 min. For the experiment 2, the mean residence time, the
second moment (Variance) and third moment (Skewness) are 11.2060 min, -97.6774 min2
and -68.6368 respectively.

INTRODUCTION
Tubular reactors are often used when continuous operation is required but without
back-mixing of products and reactants. The Tubular Reactor is specially designed to allow
detailed study of this important process. Reactions are monitored by conductivity probe as the
conductivity of the solution changes with conversion of the reactants 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.
A cooling coil and immersion heater are provided inside the vessel to provide
constant reaction temperature. The desired reaction temperature is achieved by controlling the
heating using a digital temperature controller located on the front panel. Two non-corroding
Page 1

feed storage vessels are supplied, together with chemically resistant pumps and flowmeters.
A product collection vessel is also provided and if necessary, the products are neutralized
before discharging to the laboratory drains. The tubular reactor is a coil of long tubing
wound around a cylinder inside the vessel to give a total reactor volume of approximately 0.4
litres. The spiral design is practically the best approximation to plug flow conditions, as the
secondary flow ensures good radial mixing while minimizing longitudinal dispersion. The
two reactants are pre-heated prior to mixing and entering the reactor.

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

THEORY
Like in another reactor, in tubular reactor, feed will enter the reactor from one end of the
cylindrical tank and the product stream leaves at the other end. Because of the tank will be in
a long cylindrical shape and lack of provision, then the mixing will be not in complete. Thus,
the flowing stream will vary from one point to another point.
In ideal tubular reactor, there are few specific assumptions can be made.

no mixing in the axial direction

complete mixing in the radial direction

a uniform velocity profile across the radius

Page 2

Figure 1: Tubular Reactor

The tubular flow rate reactor at steady state, the general mole balance is as stated below,

FA (y) FA (y + y) + r V = 0

(1)

Where FA (y) = molar flow rate of A

FA (y + y) = molar flow rate of A out of the volume
rA = function of reactant concentration
V = volume of reactor, which is the product of cross-sectional area of reactor and
the length of reactor;
V = Ay

(2)

Substituting equation (1) and (2),

-

( )

] = -ArA

Taking the limit of y to zero,

( )

)
Page 3

It is usually most convenient to have the reactor volume, V rather than the reactor
length, y as the independent variable. Accordingly, the variables Ady can be changed to dV
to obtain this form of the design equation for a tubular flow reactor.
The residence time distribution of a tubular flow rate reactor is a characteristic of the
mixing that occurs in the chemical reactor. The continuous stirred tank reactor (CSTR) is
thoroughly mixed and possesses a far different kind of residence time distribution (RTD) than
the plug flow reactor. The RTD is determined experimentally by injecting an inert chemical
called a tracer into the reactor at some time t=0 and then measuring the tracer concentration,
C in the effluent stream as function of time. The two methods of injection are pulse input and
step input.
In a pulse input, an amount of tracer, No is injected in one shot into the feed stream
entering the reactor in as short time possible. The outlet concentration is measured as
function of time. The effluent concentration vs. time is referred to as C(t) curve in RTD
analysis. Consider the injection of a tracer pulse for single input and output system in which
only flow that does not have dispersion carries the tracer material across system boundaries.
For a small time increment ( t) that the concentration of tracer is essentially constant, the
amount of tracer C(t) exiting between time t and (t + t) is,
N = C(t)vt

(3)

where v = effluent volumetric flow rate

To simplify it, N is the amount of material that has spent in amount of time between t and (t
+ t) in the reactor. If it is divided by total amount of material that was injected into the
reactor, No
( )

which represent the fraction of the material that has residence time in the reactor between
time t and (t + t). For example,

Page 4

Figure 2: Residence Time Distribution Function

For pulse injection,

E(t) =

( )

(4)

( )
Where E(t) = residence time distribution function
It is the function that describes in a quantitative manner how much time different
fluids elements have spent in the reactor. If No can be determined from the outlet
concentration measurement by summing up all the amounts of materials,

between time t

= 0 and infinity. Equation (3) can be written in differential form,

dN= C(t)vdt

(5)

Integrating equation (5)

No =

( )

The volumetric flow rate, v is usually constant, so that by substituting equation (5) into
equation (4), E(t) can be defined as

Page 5

E(t) =

( )

( )

The integral in the denominator is the area under the C(t) curve.

APPARATUS

Figure 3: Tubular Flow Reactor

PROCEDURE
1. The general set-up is performed.
a. All valves are initially closed except valve V7.
b. Water de-ionizer is connected to the laboratory water supply.
c. Power for control panel is turned on.
d. Water jacket B4 is assured to be filled and B5 is preheated with clean water.
Valves V13 and V8 are opened. Pump P3 is switched on to circulate the water
through pre-heated B5.
e. Stirrer motor M1 is switched on and the speed is set at about 200 rpm.
f. Valves V2 and V10 are opened. Pump P1 is switched on and the flow rate is
adjusted to 700 ml/min at flow meter FI-01. Valve V10 is closed and pump P1
is switched off.
Page 6

2. Valve V9 is opened and pump P1 is switched 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 FI-01.
4. The de-ionized water is let to continue flowing through the reactor until the inlet (QI01) 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. Valve V11 is opened and pump P2 is switched 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 700ml/min at F1-02.
8. The salt solution is let to flow for 1 minute, and then the timer is reset and restarted.
The time will be started at the average pulse input.
9. Valve V11 is closed and pump P2 is switched off. Then, valve V9 is quickly opened
and pump P1 is switched on.
10. The de-ionized water flow rate is assured to always maintained at 700 ml/min by
adjusting P1 flow controller.
11. Both inlet (QI-01) and outlet (Q1-02) conductivity values are started to be recorded at
regular intervals of 30 seconds.
12. The recording of values is continued until all readings are almost constant and
approached the stable low level values.

RESULT
Experiment 1: Pulse input
Table 1: Pulse input in tubular flow reactor
Time (min)

Conductivity (ms/cm)

Inlet

Outlet

0.2

0.5

0.5

0.2

0.5

1.0

0.2

0.5

1.5

0.1

2.2

Page 7

2.0

0.1

0.6

2.5

0.1

0.2

3.0

0.1

0.1

3.5

0.1

0.1

4.0

0.1

4.5

Outlet Conductivity vs Time

Outlet Conductivity (ms/cm)

2.5
2
1.5
1
0.5
0
0

0.5

1.5

2.5

3.5

4.5

Time (min)
Figure 4: Graph of c(t) vs time

Table 2: Conductivity value for pulse input

Time
(Min)

Conductivity
(ms/cm)

E(t)

tE(t)

(t-tm)

(t-tm)2
E(t)

t E(t)

(t -tm)

(t-tm)3
E(t)

Inlet

Outlet

0.2

0.5

0.1

2.161

0.216

0.0

-3.177

-0.318

0.5

0.2

0.5

0.1

0.05

0.941

0.094

0.025

-0.913

-0.091

1.0

0.2

0.5

0.1

0.1

0.221

0.022

0.1

-0.104

-0.010

1.5

0.1

2.2

0.44

0.66

0.0009 0.000396

0.99

2.7x10-5

1.2x10-5

Page 8

2.0

0.1

0.6

0.12

0.24

0.281

0.034

0.48

0.149

0.018

2.5

0.1

0.2

0.04

0.1

1.061

0.042

0.25

1.093

0.044

3.0

0.1

0.1

0.02

0.06

2.341

0.047

0.18

3.582

0.072

3.5

0.1

0.1

0.02

0.07

4.121

0.082

0.245

8.365

0.167

4.0

0.0

0.1

0.02

0.08

6.401

0.128

0.32

16.194

0.324

4.5

0.0

0.0

0.0

0.0

9.181

0.0

0.0

27.818

0.0

E(t) vs time
0.5
0.45

0.44

0.4
0.35

E(t)

0.3
0.25
0.2
0.15
0.1

0.1

0.1

0.12

0.1

0.05

0.04

0.02

0
0

0.5

1.5

2.5

0.02
3.5

0.02
4

0
4.5

Time (min)

Figure 5: Residence time distribution function

Experiment 2: Step change input

Flow rate = 700 mL/min
Table 3: Step change input in tubular flow reactor
Time (min)

Conductivity (ms/cm)

Inlet

Outlet

0.5

3.1

1.0

3.4

0
Page 9

1.5

3.5

2.0

3.5

2.5

3.5

0.4

3.0

3.5

1.7

3.5

3.5

2.1

4.0

3.5

2.1

4.5

3.5

2.2

5.0

3.5

2.2

5.5

3.5

2.2

Table 4: Conductivity value for step change input

Time
(Min)

Conductivity
(ms/cm)

F(t)

E(t)

tE(t)

(t-tm)3

t E(t)

(t -tm)

-1407.19

1369.475

-1227.1

405.2514

0.1858

-1063.08

-197.521

E(t)

Inlet

Outlet

0.0

0.0

0.0

0.0000

0.9732 0.0000

0.0000

0.5

3.1

0.0

0.0000

-0.3303

-0.1651

-0.0826

1.0

3.4

0.0

0.0000

0.1858

0.1858

1.5

3.5

0.0

0.0000

0.5750

0.8624

1.2936

-914.368

-525.716

2.0

3.5

0.0

0.0000

0.8372

1.6744

3.3488

-780.213

-653.194

2.5

3.5

0.4

0.1818

0.9726

2.4314

6.0784

-659.866

-641.753

3.0

3.5

1.7

0.7727

2.943

8.829

-552.579

-542.08

3.5

3.5

2.1

0.9545

3.0189

10.5662

-457.601

-394.704

0.981

0.8626

Page 10

4.0

3.5

2.1

0.9545

0.6172

2.4688

9.8752

-374.182

-230.945

4.5

3.5

2.2

1.0000

0.2450

1.1023

4.9602

-301.572

-73.87

5.0

3.5

2.2

1.0000

-0.2542

-1.271

-6.355

-239.021

60.75903

5.5

3.5

2.2

1.0000

-4.8414

-26.6276

-185.778

163.5315

-0.8803

Outlet conductivity vs time

3

Conductivity (ms/cm)

2.5
y = -0.0846x3 + 0.7064x2 - 0.9732x + 0.1454
2

2.1

2.1

2.2

2.2

2.2

1.7

1.5
1
0.5

0.4

0
-0.5
-1

0
0

0
1

0
2

time (min)

Figure 6: Graph of Outlet conductivity vs time

Page 11

E(t) vs time
1.5
1
0.8372

0.972550.981

0.86255
0.6172

0.57495

0.5

0.24495

E(t)

0.1858
0
0

1
-0.33025

-0.5
-1

5 -0.2542

-0.88025

-0.9732

-1.5

time (min)

Figure 7: Residence Time Distribution (RTD) function

SAMPLE OF CALCULATION
Experiment 1: Pulse input in tubular flow reactor
Residence time distribution function, E(t)
( )

h=

tN - t0 8 - 0
=
=1
N
8

C(t)dt =
0

(t) =

(t) =

1 0.5 + 4(0.5) + 2(0.5) + 4(2.2) + 2( ) + 4(0.2)

[
] =
+ 2(0.1)+ (0.1) ( )
3

C(t)
8
0 C(t)dt

0
=
15.0 m .min/m
Page 12

Mean residence time, tm

N

(t)dx =

h
3

+4

1+

+4

+2 +

.. + 4

N-1

tm = t (t)dt
0

1 0 +4(0.05) + 2(0.1) + 4(0.66) + 2(0.24) + 4(0.1) + 2(0.06) + 4(0.07)

[
]
3
+ 0. 8

min

Second moment, variance, 2

2

= ( t- tm )2

(t) dt

= t2 (t) dt - 2tm t (t)dt +

0

tm 2 (t) dt

= t2 (t) dt - 2tm 2 + tm 2
0

= t2 (t) dt - tm 2
0

t2 (t) dt =
0

1 0 + 4(0.025) + 2(0.1) + 4(0.99) + 2(0.48) + 4(0.25) + 2(0.18)

[
]
+ 4(0.245)+0
3
= 2.6267 min2

= t2 (t) dt - tm2
0

= 2.6267 min2 - (

min)2

= 0.4756 min2

Page 13

Third moment, skewness, s3

3

(t - tm )3 (t) dt

3
2

(t - tm )3 (t) dt
0

1 -0.3
[
3

+ 4(-0.091) + 2(-0.010) + 4(1.2x10 -5) + 2(0.018) + 4(0.044) + 2(0.072) +

]
4(0.16 ) + 0.324

= 0.2145

=0.4756 min2 = 0.6896 min

3

3
2

(t - tm )3 (t) dt =
0

1
3

(0.6896) 2

) = 0.3746

Experiment 2: Step change input in tubular flow reactor

(t) =

C(t)
C0
0 m /cm
2.2 m /cm

=
(t) =
=

d
dt

d C(t)
dt C0

(y = -0.0846 t3 + 0.7064 t2 - 0.9732 t + 0.1454 )

= -0.2538 t2 + 1.4128 t - 0.9732 , substitute each of the value of time (min)

= -0.2538(0)2 + 1.4128(0) 0.9732
= 0.9732

Page 14

Mean residence time, tm

N

(t)dx =

h
3

+4

1+

+4

+2 +

.. + 4

N-1

11

tm = t (t)dt
0

0 +4 (-0.16513) + 2(0.1858) + 4 (0.86242) + 2 (1.6744) + 4 (2.431375) + 2(2.943)

+ 4(3.018925) + 2(2.4688) + 4(1.102275) + (-1.271)

-4.84138

tm = 11.2060 min

Second moment, variance, 2

2

= ( t- tm )2

(t) dt

= t2 (t) dt - 2tm t (t)dt +

0

tm 2 (t) dt

= t2 (t) dt - 2tm 2 + tm 2
0

= t2 (t) dt - tm 2
0

t2 (t) dt =
0

1
0 + 4(-0.0826) + 2(
3
+ 4(

) + 2(

) + 4(
) + 4(

) + 2(
) + 4(

) + 4(

) + 2(

)+

= 27.898 min2

11

= t2 (t) dt - tm2
0

min2 - (

min)2

Page 15

= -97.6774 min2

Third moment, skewness, s3

3

3
2

(t - tm )3 (t) dt
0

11

(t - tm )3 (t) dt
0

) + 4(-525.716) + 2(-653.194) + 4(-641.753)

1369.475+ 4(405.2514) + 2(

+ 2(-542.08)+ 4(-394.704) + 2(-230.945) + 4(-73.87) + (

= -2131.53
=
3

min2 = 9.88 min

1
3
2

11

3
0 (t - tm ) (t) dt =

1
(

3
) 2

) = -68.6368

DISCUSSION
Experiment 1 has showed the effect of the pulse input and experiment 2 has showed
the effect of step change input to the tubular flow reactor. A pulse input is when known mass
of chemical is added into the system at all once. Monitoring for the chemical at the reactor
outlet begins at the same time as the addition of pulse. While for step change input, the
known of chemical mass is added continuously into the reactor during the reaction.
From the graph of Residence Time Distribution (RTD), it showed difference in
experiment 1 and 2. In experiment 1, the E(t) values are constant at the first, then, the values
increased by time. After that, it decreased by time and the values become constant at last. For
experiment 2, the values of E(t) increased and then it decreased. It did not achieve any
constant values. Residence time distribution is referring to any fluid (plug) that enters the
reactor at time t will exit the reactor at time t + , where is the residence time of the reactor.
Residence time in the reactor is equal to the space time if the conditions in the reactor like
Page 16

pressure and temperature are same as those at the entrance. We use the RTD concept as we
know that when any feed enter the reactor, the product that exit the stream is not in the same
amount of time. This is due to the turbulent mixing as when these situations occur, some of
the molecules will find their way out rapidly while some of the molecules will spend more
time inside the reactor before they exit through the stream.
The RTD of a real reactor deviate 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 non-uniform velocity
profile, or diffusion. If the mean of the

curve arrives earlier than the expected time

it indicates that there is stagnant fluid within the vessel. If the RTD curve shows more than
one main peak it may indicate channelling, parallel paths to the exit, or strong internal
circulation. A step experiment is often easier to perform than a pulse experiment, but it tends
to smooth over some of the details that a pulse response could show. It is easy to numerically
integrate an experimental pulse response to obtain a very high-quality estimate of the step
response, but the reverse is not the case because any noise in the concentration measurement
will be amplified by numeric differentiation.
Once we got the values of the inlet and outlet conductivity, the graph of outlet
conductivity vs time is plot where this graph is also known as C(t) curve. The amount of C(t)
is later is then being integrate before being used to obtain the value of E(t). Once we obtain
the readings of E(t), graph of E(t) vs time is plot and this is also known as the residence time
distribution (RTD) function for the reactor. For the first experiment, the value of mean
residence time is 1.4667 min, the second moment (Variance) is 0.4756 min2 and the third
moment (Skewness) is 0.3746 min. For the experiment 2, the mean residence time, the
second moment (Variance) and third moment (Skewness) are 11.2060 min, -97.6774 min2
and -68.6368 respectively. In this experiment, it can be seen that pulse input and step change in
tubular reactor method has a few differences. For pulse input method, it can be seen the inlet
tracer concentration is suddenly change from 0.2 to the 0.1 and return it to zero after a short
time. While for the step input change method the feed tracer is suddenly changed from zero
to steady value at Ct after time reached to zero.
The curve E(t) is observe by calculating the area under the graph. For E(t) curve pulse
input and step change input, they are not so in bell-shaped and this is different from the
theory). This may causing the readings are wrong and cause the graph to be not following the
Page 17

theory. However, based on the graph, we still can see the flow is increasing before decreasing
and there is also a steady state throughout the reactor .

CONCLUSION
The first experiment was conducted to examine the effect of a pulse input in
tubular flow reactor and to construct a residence time distribution (RTD) function for the
tubular reactor. While the second objective for experiment 2 is to examine the effect of a step
change input in tubular flow reactor and to construct a residence time distribution (RTD)
function for the tubular flow reactor. From the graph of first experiment, we
can be see that the residence time distribution (RTD) for pulse input increased with time.
However after a few minutes, it will slowly decreases until the value of zero. For the second
experiment, it can be seen that the value slowly increase of outlet conductivity and E(t) until
the outlet conductivity is constant. The mean residence time, second moment (Variance) and
third moment (Skewness) were calculated was calculated from the graph. For the first
experiment, the value of mean residence time is 1.4667 min, the second moment (Variance)
is 0.4756 min2 and the third moment (Skewness) is 0.3746 min. For the experiment 2, the
mean residence time, the second moment (Variance) and third moment (Skewness) are
11.2060 min, -97.6774 min2 and -68.6368 respectively.

RECOMMENDATION
1) Make sure Tank 1 and Tank 2 are full with sodium chloride and deionised water to
avoid running out of salt solution.
2) Make sure that the valve is open or close according to the general start-up procedure.
3) Ensure that there are no leakages at the valve to prevent it from effecting the result of
the experiment.
4) If the students manage to have enough time, do more trial to get average of
conductivity for both inlet and outlet conductivity values in order to get more accurate
results for both experiments.

Page 18

REFERENCES
1) Fogler H and Gurmen N (2008) Element of Chemical Reaction Engineering Retrieved
from http://www.engin.umich.edu/~cre/344/lecnotes.htm on 10 April 2012.
2) Gilmour D and Samson P (1992). Reaction Kinetics. Retrieved from
http://www.colorado.edu/che/courses/chen4130/documents/TubularFlowReactorOper
ationInstructions.pdf on 10 April 2012.
3) Hatzikiosiyian P. and Remoundaki S. (2003) Residence Times in Mixed Tanks and a
Tubular Reactor Retrieved from
http://cbi.izt.uam.mx/iq/Manuales%20de%20Equipos/REACTORES/CET%20MKII
%20TUBULAR%20REACTOR.pdf on 10 April 2012.
4) Residence Time Residence (RTD) Retrieved from
http://en.wikipedia.org/wiki/Residence_time_distribution on 10 April 2012.
5) Resources Gold Technology (2006) Gold Leaching Equipment Retrieved from
http://www.resourcesgoldtechnology.com/gold-leaching-equipment.html on 10 April
2012.
6) (n.d). Retrieved from
http://solve.nitk.ac.in/dmdocuments/Chemical/theory_plugflow.pdf
7) (n.d). Retrieved from
http://www.neduet.edu.pk/Chemical/PDF/CHEMICAL%20REACTION%20ENGINE
ERING%20LAB.pdf
8) (n.d). Equipment for Engineering Education & Research, Tubular Flow Reactor
http://www.solution.com.my/pdf/BP101(A4).pdf

APPENDIX

Page 19