ABSTRACT

Residence time distribution is measured experimentally by use of an inert tracer

injected into the reactor at t=0.The method of injection used is pulse input and step change
input .The experiment is conducted to achieve the 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. For the both input experiment, the flow rate was set up at 700 m3s-1and 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 is constant for 3 times.

INTRODUCTION
Tubular flow reactor (TFR) also known as plug flow reactor is a vessel through which
flow is continuous and usually at steady state. This type of reactor commonly used in industry.
It is consist cylindrical pipe and mostly operated at gas phase reaction. In the tubular flow
reactor, the reactants are continually consumed as they flow down the length of the reactor. In
modelling the tubular reactor, we assume the concentration varies continuously in the axial
direction through the reactor. Consequently, the reaction rate, which is a function of
concentration for all but zero order reactions, will also vary axially.
There are tubular flow reactors applications which are :

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions

The residence time distribution (RTD) of a chemical reactor is a probability distribution

function that describes the amount of time a fluid element could spend inside the reactor.
Chemical engineers use the RTD to characterize the mixing and flow within reactors and to
compare the behavior of real reactors to their ideal models. This is useful, not only for
troubleshooting existing reactors, but in estimating the yield of a given reaction and designing
future reactors.
OBJECTIVES
1. To examine the effect of a pulse input in a 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
The theory of residence time distributions 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
3. the flow is incompressible.

Residence time distributions (RTD) are used to model the imperfect mixing behaviour of real
reactors. RTD can be determined experimentally by injecting an inert chemical, molecule, or
atom, called tracer, into the reactor at some time t=0 and then measuring the tracer
concentration C in the exit stream as a function of time. Pulse and step inputs are the two
commonly used methods of injection.
Pulse input
This method required the introduction of a very small volume of concentrated tracer at the inlet
of the reactor,such that it approaches the dirac delta function.Although an infinitely short
injection cannot be produced.It can be made much smaller that the residence time of the
vessel.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 the following relation :

E(t) =

()

0 ()

Step change input

Just as the RTD function E(t) can be determined directly from a pulse input, the cumulative
distribution F(t) can be determined directly from a step input .By analyzing a step input in the
tracer concentration for a system with a constant volumetric flow rate. Consider a constant rate
of tracer addition to a feed that is initiated at time t = 0. Before this time no tracer was added
to the feed. The concentration of tracer in the feed to the reactor is kept at this level until the
concentration in the effluent is indistinguishable from that in the feed; the test may then be
discontinued.RTD function can be obtained by the following relation :
E(t) =

()

PROCEDURE
General start-up procedure

1. All valves were ensured initially closed except valve V7.

2. 20 litre of salt solution was prepared. For example, sodium chloride,
NaCl(0.025M).
3. The food tank B2 was filled with the NaCl solution.
4. The power for the control panel was turned up.
5. The water deionizer was connected to the laboratory water supply. Valve V3
was opened and feed tank B1 was filled up with the deionized water. Valve V3
was closed.
6. Valves V2 and V10 were opened. Pump P1 was switched on P1 flow controller
was adjusted to obtain a flow rate of approximately 700ml/min at flow meter
F1-01. The conductivity display was observed at low value then a valve V10was
closed and pump P1 was switched off.
7. Valves V6 and V12 were opened. Pump P2 was switched on. P2 flow controller
was adjusted to obtain a flow rate of approximately 700 ml/min at flow meter
F1-02. A valve V12 was closed and pump P2 was switched off.
8. The unit was ready for experiment.

General shut-down procedures

1. Both pump P1, P2 and P3 were switched off. Valves V2 and V6 wre closed.
2. The heaters were switched off.
3. The cooling water was kept circulating through the reactor while the stirrer
motor is running to allow the water jacket to cool down to room temperature.
4. All liquid were drained from the unit by opening valves V1 and V16 if the
equipment is not going to be used for long period of time. The feed tanks were
rinsed with clean water.
5. The power for the control panel was turned off.

Experiment 1 : Pulse 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 controller is adjusted to give a constant flow rate of de-ionized water into
the reactor R1 at approximately 700 ml/min at Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Ql-01)
and outlet (Ql-02) conductivity values are stable at low levels. Both conductivities values
are recorded.
5. Valve V9 is closed and pump P1 is switch off.
6. Valve V11 is opened and Pump P2 is switch 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 700 ml/min at Fl-02.
8. Let the salt solution to flow for 1 minute, then reset and restart the timer. This will start
the time at the average pulse input.
9. Valve V11 is closed and pump P2 is switch off. Then, open valve V9 quickly and
pumpP1 is switch on.
10. Make sure that the de-ionized water flow rate is always maintained at 700 ml/min by
adjusting P1 flow controller.
11. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular intervals of 30
seconds is start recorded.
12. The conductivity values is continue recording until all readings are almost constant and
approach 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 switch 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 Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Ql-01)
and outlet (Ql-02) conductivity values are stable at low levels. Both conductivities values
are recorded.
5. Valve V9 is closed and pump P1 is switch off.
6. Valve V11 is opened and Pump P2 is switch on. The timer is started simultaneously.
7. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular intervals of
30seconds is start recorded.
8. The conductivity values is continue recording until all readings are almost constant

Preparation of Calibration Curve for Conversion vs Conductivity:

1. The following solution were prepared:

1 L of sodium hydroxide, NaOH (0.1M)

1 L of sodium acetate , Et (Ac) (0.1M)

1 L of deionised water, H2O

2 The conductivity and NaOH concentration for each value were determined by mixing the
following solution into 100 mL of deionised water

0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL Et (Ac)

50% conversion : 50 mL NaOH + 50 mL Et (Ac)

75% conversion : 23 mL NaOH + 75 mL Et (Ac)

100% conversion : 100 mL Et (Ac)

APPARATUS AND MATERIALS

-Tubular flow reactor
-Deionized water
-Sodium hydroxide
-Ethyl acetate

RESULT
Experiment 1 : Pulse input in a Tubular flow reactor
Flowrate : 700ml/min
Type of input : Pulse input
Time (min)

Conductivity (mS/cm)
Inlet

Outlet

0.0

3.0

0.0

0.5

0.3

0.0

1.0

0.1

2.5

1.5

0.0

2.3

2.0

0.0

0.4

2.5

0.0

0.0

3.0

0.0

0.0

3.5

0.0

0.0

4.0

0.0

0.0

4.5

0.0

0.0

5.0

0.0

0.0

Table 1

Outlet conductivity vs time

Outlet conductivity (mS/cm)

3
2.5
2
1.5
1
0.5
0
0
-0.5

Time(min)

Graph 1

Experiment 2 : Step change in a Tubular Flow Reactor

Flowrate : 700ml/min
Type of input : Step change input
Time (min)

Conductivity (mS/cm)
Inlet

Outlet

0.0

0.0

0.0

0.5

3.3

0.0

1.0

3.6

0.0

1.5

3.7

0.0

2.0

3.7

1.6

2.5

3.8

4.4

3.0

3.8

4.9

3.5

3.9

4.9

4.0

3.9

4.9

4.5

3.9

4.9

5.0

3.9

4.9

Table 2

Outlet conductivity vs Time

Outlet conductivity (mS/cm)

6
5
4
3
2
1
0
0
-1

Time (min)

Graph 2

PREPARATION OF CALIBRATION CURVE

Conversion

Solution Mixtures

Concentration Conductivity
of NaOH

H2 O

(ms/cm)

0.1 M

0.1 M

NaOH

Et(Ac)

0%

100 mL

100 mL

0.0500

5.64

25%

75 mL

25 mL

100 mL

0.0375

4.35

50%

50 mL

50 mL

100 mL

0.0250

3.70

75%

25 mL

75 mL

100 mL

0.0125

3.39

100%

100 mL

100 mL

0.0000

7.42 x 10^-5

(M)

Table 3

Conductivity vs Conversion
7

Conductivity (mS/cm)

6
5
4
3
2
1

y = -4.896x + 5.864

0
0%

20%

40%

60%

80%

100%

120%

Conversion (%)

Graph 3

10

SAMPLE CALCULATION
Experiment 1 : Pulse input in a Tubular flow reactor

0 () = Area under the graph

(1)+(2)

Area = (t2 t1)(

Time (0.5-1.0) minutes

Area = (1.0 0.5)(

0+2.5
2

= 0.625 g.min/m3

Time (1.0-1.5) minutes

Area = (1.5 1.0)(

2.5+2.3
2

= 1.2 g.min/m3

Time (1.5-2.0) minutes

Area = (2.0 1.5)(

2.3+0.4
2

= 0.675 g.min/m3

Time (2.0-2.5) minutes

Area = (2.5 2.0)(

0.4+0.0
2

= 0.1 g.min/m3

:: So the total area

5

0 () = (0.625 + 1.2 + 0.675 + 0.1) = 2.6

E(t) =

()

0 ()

11

For t=0, C(t) = 0.0

E(t) = 0/2.6
=0

For t=0.5, C(t) = 0.0

E(t) = 0/2.6
=0

For t=1.0, C(t) = 2.5

E(t) = 2.5/2.6
= 0.962

For t=1.5, C(t) = 2.3

E(t) = 2.3/2.6
= 0.885

For t=2.0, C(t) = 0.4

E(t) = 0.4/2.6
= 0.154

For t=2.5 5.0, C(t) = 0

E(t) = 0/2.6
=0

12

Time(min)

Outlet conductivity (mS/cm)

E(t)

0.0

0.0

0.0

0.5

0.0

0.0

1.0

2.5

0.962

1.5

2.3

0.885

2.0

0.4

0.154

2.5

0.0

0.0

3.0

0.0

0.0

3.5

0.0

0.0

4.0

0.0

0.0

4.5

0.0

0.0

5.0

0.0

0.0

Table 1.1

E(t) vs Time
1.2
1

E(t)

0.8
0.6
0.4
0.2
0
0
-0.2

10

12

Time(min)

Graph 1.1 ; Residence time distribution (RTD) for plug flow reactor

13

For time (0-0.5)min = 0

For time (0.5 -1.0) minutes

(1+2)

Area = (t2 t1)(

= (1.0 -0.5) (

0.962

=0.2405

For time (1.0 -1.5) minutes

Area= (1.5 -1.0) (

0.962+0.885
2

=0.462

For time (1.5 -2.0) minutes

Area= (2.0 -1.5) (

0.885+0.154
2

=0.260

For time (2.0 -2.5) minutes

Area= (2.5 -2.0) (

0.154
2

=0.039

For time (2.5-5.0)min = 0

0 () = Total area under the graph = (0.2405+ 0.462 + 0.260+ 0.039)

=1.0015

Residence time.tm =0 ()
= 5(1.0015)
=5.008

14

Time(min)

Outlet

E(t)

(t-tm)2() (t-tm)3()

tE(t)

conductivity
(mS/cm)
0.0

0.0

0.0

0.0

0.0

0.0

0.5

0.0

0.0

0.0

0.0

0.0

1.0

2.5

0.962

0.962

15.454

-61.938

1.5

2.3

0.885

1.328

10.890

-38.205

2.0

0.4

0.154

0.308

1.393

-4.191

2.5

0.0

0.0

0.0

0.0

0.0

3.0

0.0

0.0

0.0

0.0

0.0

3.5

0.0

0.0

0.0

0.0

0.0

4.0

0.0

0.0

0.0

0.0

0.0

4.5

0.0

0.0

0.0

0.0

0.0

5.0

0.0

0.0

0.0

0.0

0.0

=2.001

= 2.598

=27.737

=-104.334

Mean residence time, tm 0 () = 2.001

Second moment,Variance, 20 (t-tm)2() = 27.737

3

Third moment,Skewness,s3 1/^(2) 0

(t-tm)3() = -8.632

15

Experiment 2 ; Step change input in a Tubular Flow Reactor

Time

Conductivity

(min)

(mS/cm)
Inlet

Outlet

C(t)

E(t)

tm

s3

Ci(t)

Ci(t)/ Ci(t)

t*E(t)/Ci(t)

(t-tm)2 *

(t-tm)3 *

E(t)/Ci(t)

E(t)/Ci(t)

0.0

0.0

0.0

0.0

0.0

0.0

0.0

0.0

0.5

3.3

0.0

0.0

0.0

0.0

0.0

0.0

1.0

3.6

0.0

0.0

0.0

0.0

0.0

0.0

1.5

3.7

0.0

0.0

0.0

0.0

0.0

0.0

2.0

3.7

1.6

0.4

0.0285

0.004

0.008

0.016

2.5

3.8

4.4

1.5

0.1069

0.019

0.047

0.116

3.0

3.8

4.9

2.33

0.1661

0.036

0.104

0.308

3.5

3.9

4.9

2.45

0.1746

0.044

0.149

0.514

4.0

3.9

4.9

2.45

0.1746

0.050

0.194

0.767

4.5

3.9

4.9

2.45

0.1746

0.056

0.246

1.092

5.0

3.9

4.9

2.45

0.1746

0.062

0.306

1.498

=0.2710

=1.054

=4.311

=14.03

=0.9999

Table 2.1

E(t) vs Time
0.2
0.18
0.16
0.14

E(t)

0.12
0.1
0.08
0.06
0.04
0.02
0
-0.02

3
Time(min)

Graph 2.1 Residence time distribution (RTD) graph

16

0 () = Ci(t) =Area
Based on the table we calculated, the total area is = 14.03m2
For t=2.0 min
tm =
=

()

2.0 0.0285
14.03

= 0.004
2 = (t-tm)2 E(t) /Area
= (2.0 0.004)2(0.0285) / 14.03
=0.008
s3 = (t-tm)3 E(t) /Area
= (2.0 0.004)3(0.0285) / 14.03
=0.016

Mean residence time, tm 0 () = 0.2710

Second moment,Variance, 20 (t-tm)2() = 1.054

3

Third moment,Skewness,s3 1/^(2) 0

(t-tm)3() = 4.144

17

DISCUSSION
The purpose of this experiment is to study the effect of a pulse input and effect of a step
change input in a tubular flow reactor.The result obtained for each input were calculated and
the graph of residence distribution time for each input have been plotted.
For the experiment 1,which is pulse input. In a pulse input, an amount of tracer No is
suddenly injected in one shot into the feed stream entering the reactor in as short time as
possible. The result obtained is recorder in table 1 and the graph is plotted. The table 1 shows
that when time is zero, the outlet conductivity is zero but at the time t=1 min , the outlet
conductivity recorded is 2.5mS/cm. At this time the rate of reaction start to decrease to
0.4mS/cm at t=2 min. The rate of reaction is decrease to zero from t=2.5min until t=5min,this
is because all the reactant is fully consumed. Based on the graph 1, area under the graph is
calculated then graph 1.1 residence time distribution (RTD) been plotted. From the RTD graph
the highest peak is at t=2.5min .
For the pulse input,the residence time calculate is 5.008 . There are 3 data that had been
obtained and calculated which are mean residence time ,variance (second moment),2 and
skewness (third moment),s3 that recorded 2.001, 27.737 and -8.632 respectively. The skewness
for the pulse input give a negative value and it called negative skew.
The experiment 2 is the study of step change input, The graph 2 of step change shows
the outlet conductivity is increase within the time by started at time of 2.0 minutes which it
inlet conductivity is 1.6 mS/min and then undergoes some increment until at minutes 5.0 which
the outlet conductivity is 4.9mS/min. There are differences between both of the graph where
the outlet conductivity for step change is increase smoothly compare to pulse input where the
outlet conductivity is increase at the some period of times and then it become decrease into the
constant value.
For the step change, the graph indicate almost same to the outlet conductivity versus
time which the residence time distribution (RTD) is increase within the time. The mean
residence time distribution that calculated is 0.2710minutes. The other 2 data are also need to
be calculate which are variance (second moment), 2 and skewness (third moment), s3 are
1.054and 4.144 respectively. The skewness give a positive value and it called positive skew
compare to pulse input.

18

For the preparation calibration curve, the graph of conductivity vs conversion is been
plotted based on table 3. Graph conductivity vs conversion shows the trend decreasing from
0% to 50% conversion, The conductivity start to increase from 50% to approaching 80%
conversion but the conductivity start to increase by 78% conversion until complete
conversion. The table 3 shows that the concentration of NaOH decrease as the reaction
proceeds which resulting the decrease in conductivity value.This graph shows the trend
negative slope which is -4.896.
CONCLUSION
In a nutshell. from the experiment we are able to study the effect of the pulse input an
and step change input in a tubular flow rate and we also can compared the both effect.The
residence distribution graph (RTD) function also be able to construct for the tubular flow
reactor
For the pulse input type, the outlet conductivity is at the peak when time at t=1.0 min
which is 2.5mS/cm. The graph RTD function with distribution of time,E(t) vs time is been
plotted. The residence time can be calculated from graph using area under graph,so the
residence time, tm is 5.008.The mean residence time is 2.001.The variance and skewness also
been calculated which are 27.737 and -8.632.
Step change input,the graph 2 show outlet conductivity reach steady state at t=3min.
The graph RTD function with distribution of time,E(t) vs time is been plotted. The mean
residence time is calculated which is 0.2710.The variance and skewness also been calculated
which are 1.054 and -4.144. Thus,it can be conclude that both input when the graph plotted
almost the same as the theory which stated that exit time, E (t) is depends on the value of C (t).
RECOMMENDATION

Each experiment we must do the start-up and shut-down experiment first in order to
make sure there are no left over in the chamber.

Open and close the valve carefully according to the procedure given.

The experiment should be conducted at the stable and unshaken place.

Make sure there are no leakages at the equipment

Always alert with the time record.

19

REFERENCES
Dane.K,(2007)Non ideal reactor mixing pattern .Retrieved from
https://ocw.mit.edu/courses/chemical-engineering/10-37-chemical-and-biologicalreaction-engineering-spring-2007/lecture-notes/lec10_03092007_w.pdf

Residence time distribution.Retrieved from

http://www.che.iitb.ac.in/courses/uglab/cl431/ms401-rtd.pdf

Nauman, E. Bruce (2004). Residence Time Distributions. Retrieved from

https://en.wikipedia.org/wiki/Residence_time_distribution

H. Scott Fogler,(2004) Elements of Chemical Reaction Engineering Fourth Edition.

Pearson

Residence time distribution in Chemical Reactor.Retrieved from

http://www.slideshare.net/narendrakumard/rtd-8786036

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