UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY III
(CHE574)
NAME
STUDENT NO.
GROUP
EXPERIMENT
DATE PERFORMED
SEMESTER
PROGRAMME / CODE
SUBMITTED TO
No.
1
2
3
4
5
6
7
8
9
10
11
12

Title
Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference / Appendix
TOTAL MARKS

Remarks:
Checked by :
--------------------------Date :
1.0

ABSTRACT

: NUR AFIQAH BINTI ANUWAR

: 2013279908
: EH2204 ( GROUP 4 )
: TUBULAR FLOW REACTOR
: 9 APRIL 2015
:4
: EH2204A
: SITI KHATIJAH JAMALUDIN
Allocated Marks (%)
5
5
5
5
5
10
10
10
20
10
5
10
100

Marks

The experiment was divided into two parts which are Experiment 1 : Pulse Input in a
Tubular Flow Reactor and Experiment 2 : Step Change Input in a Tubular Flow Reactor.
In Experiment 1 the objective of the experiment is to examine the effect of a pulse input
in a tubular flow reactor while in Experiment 2, the objective is to examine the effect of a
step change input in a tubular flow reactor. For both part of the experiment, we need to
construct a residence time distribution (RTD) function for the tubular flow reactor. The
reactor used is the SOLTEQ Tubular Flow Reactor instrument. First of all, the general
set-up procedure must be carried out before we can run the experiment. After that, we set
up the flowrate that is 700 mL/min. After the conductivity for inlet and outlet are both
reaching a constant value, the experiment is stopped. In the pulse input experiment, the
flow rate was maintained at 700 mL/min and let it for one minute before the reading were
taken every 30 seconds until the conductivity reading is 0.0. Same with experiment 1, at
the step change input experiment, the flowrate also be maintained at 700 mL/min then the
conductivity were observe every 30 seconds until the Q1 and Q2 have a constant reading
for 3 times. After all the data had been recorded, few calculations need to be done for the
further observations.

2.0

INTRODUCTION

A tubular reactor is a vessel through which flow is continuous, usually at steady state and
configured so that conversion of the chemicals are functions of position within the reactor
rather than 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. 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. Plug
flow reactors may be configured as one long tube or a number of shorter tubes. They
range in diameter from a few centimeters to several meters. The choice of diameter is
based on construction cost, pumping cost, the desired residence time and heat transfer
needs. Typically, long small diameter tubes are used with high reaction rates and larger
diameter tubes are used with slow reaction rates.
Plug flow reactors have a wide variety of applications in either gas or liquid phase
systems. Common industrial uses of tubular reactors are in gasoline production, oil
cracking, synthesis of ammonia from its elements and the oxidation of sulfur dioxide to
sulfur trioxide. Tubular reactors can also be used as bioreactors or for small scale
production.
One of the advantages of tubular flow reactor are they are easily maintained since there
are no moving parts, the conversion rate per reactor volume is high and the tubes are easy
to clean. The disadvantages are the reactors temperature is difficult to control and the
reactor itself is difficult to control due to temperature and composition variations.
Residence Time Distribution (RTD) analysis can be used to inspect the malfunction of
chemical reactors. It can also be very useful in the estimation of effluent properties and in
modeling reactor behavior. This technique is extremely important in teaching reaction
engineering, in particular when the non-ideal reactors become the issue. By impulse and
step tracer injection techniques can determine RTDs and applying them to the modeling

of the reactor flow and to the estimation of the behavior of a nonlinear chemical
transformation. 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 (FEUP). 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 (equal density, equal
viscosity) 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.

3.0

AIMS

i.

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

ii.

To examine the effect of a step change input in a tubular flow reactor.

iii.

To construct a residence time distribution (RTD) function for the tubular flow
reactor.

4.0

THEORY

In a tubular 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. In the ideal
tubular reactor which is called the plug flow reactor, specific assumptions are made
about the extent of mixing:
1. no mixing in the axial direction, i.e., the direction of flow
2. complete mixing in the radial direction
3. a uniform velocity profile across the radius.
The absence of longitudinal mixing is the special characteristics of this type of reactor. It
is an assumption at the opposite extreme from the complete mixing assumption of the
ideal stirred tank reactor.
The validity of the assumptions will depend on the geometry of the reactor and the flow
conditions.
Deviations, which are frequent but not always important, are of two kinds:
1. mixing in longitudinal direction due to vortices and turbulence
2. incomplete mixing in radial direction in laminar flow conditions

Mass Balance

For a time element t and a volume element V, the mass balance for species i is given
by the following equation:
QA CA v t- QA CAv+v t - rAVt = 0

(10.1.1)

Where QA : volumetric flow rate of reactant A to the reactor, L/s

CA : concentration of reactant A, mol/L
rA : rate of disappearance of reactant A, mol/Ls

The conversion, X, is defined as:

X = (initial concentration - final concentration) / (initial concentration)

Since the system is at steady state, the accumulation term in Equation (10.1.1) is zero.

Equation (10.1.1) can be written as:

-QA CA - rAV = 0

(10.1.2)

Dividing by V and taking limit as V 0

dCA/dV = -rA/QA

(10.1.3)

This is the relationship between concentration and size of reactor for the plug flow
reactor. Here rate is a variable, but varies with longitudinal position (volume in the
reactor, rather than with time).
Integrating,

-dV/ QA = dCA/rA

At the entrance:

(10.1.4)

V=0

CA = CA0
At the exit:

V = VR (total reactor volume)

CA = CA (exit conversion)

VR = dCA
QA

5.0

rA

APPARATUS

6.0

i.

SOLTEQ Tubular Flow Reactor instrument

ii.

Clock watch

iii.

Solution 0.025M Sodium Chloride and Deionized water.

METHADOLOGY

GENERAL START-UP
1.

All valves are initially closed except valves V7.

2.

20L of salt solution is prepared

3.

Feed tank B2 is filled with the sodium chloride solution.

4.

The ON power button is turned

5.

The water Deionizer is connected to the laboratory water supply. Valve V3

is opened and the feed tank B1 is allowed to feed with the water. Valve V3
is closed as the water level reached the tank mark.
6.

Valve V2 and V10 is opened and pump P1 is switched on. From observing
the flow meter F1-01 value, The P1 pump is adjusted by controlling the
flow controller to obtain a flow rate of approximately 700 mL/min.

7.

V6 and V12 are opened and pump 2 is switched on. From observing the
flow meter F1-02 value, The P2 pump is adjusted by controlling the flow
controller to obtain a flow rate of approximately 700 mL/min. Then the
valve V12 is closed and pump P2 is turn off.

8.

The experiment can now be carried out.

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

deionized water into the reactor R1 at approximately 700 mL/min at Fl-01.

4.

Deionized water is let 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 switched off. Then, open valve V9
quickly and pump P1 is switched on.

10.

Deionized water flow rate is make sure to 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 switched on.

3.

Pump P1 flow controller is adjusted to give a constant flow rate of

deionized water into the reactor R1 at approximately 700 mL/min at Fl-01.

4.

The deionized water is let 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 switched off.

6.

Valve V11 is opened and Pump P2 is switchd on. The timer is started
simultaneously.

7.

Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular
intervals of 30 seconds is start recorded.

8.

The conductivity values is continue recording until all readings are almost
constant.

7.0

RESULTS

Experiment 1: Pulse Input in a Tubular Flow Reactor

Flow rate

= 700 mL/min

Input type

= Pulse input

Conductivity
(mS/cm)

C(t)

E(t)

tm

s3

Ci(t)

tE(t) /

(t - tm)2

(t - tm)3

E(t) /

E(t) /

0.0000
0.0122
0.0512
0.1152
0.1948
0.1340
0.0569
0.0000
0.0000
0.5643

0.0000
0.0058
0.0483
0.1629
0.3684
0.3274
0.1696
0.0000
0.0000
1.0824

Time
(min)
Inlet

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0

Outlet

0.0
0.0
0.2
1.7
0.1
1.8
0.0
1.8
0.0
1.7
0.0
0.7
0.0
0.2
0.0
0.0
0.0
0.0
SUMMATION

Cit

Ci(t)

0.00
0.85
0.90
0.90
0.85
0.35
0.10
0.00
0.00
3.95

0.0000
0.2152
0.2278
0.2278
0.2152
0.0886
0.0253
0.0000
0.0000
0.9999
TABLE 1

0.0000
0.0272
0.0577
0.0865
0.1090
0.0561
0.0192
0.0000
0.0000
0.3557

GRAPH 1

GRAPH 2

Experiment 2: Step Change Input in a Tubular Flow Reactor

Flow rate

= 700 mL/min

Input type

= Deionized Water

Conductivity

C(t)

E(t)

tm

s3

Cit

Ci(t)

t*E(t)/

(t - tm) 2 *

(t - tm) 3 *

(mS/cm)
Time
(min)

Inlet

Outlet

Ci(t)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0

0.0
0.0
2.5
0.0
2.5
0.0
2.6
0.1
2.6
1.4
2.6
1.6
2.6
1.7
2.6
1.7
2.6
1.7
SUMMATION

0.0000
0.0000
0.0000
0.0500
0.7000
0.8000
0.8500
0.8500
0.8500
4.1000

0.0000
0.0000
0.0000
0.0122
0.1707
0.1951
0.2073
0.2073
0.2073
0.9999

TABLE 2

E(t)/
0.0000
0.0000
0.0000
0.0045
0.0833
0.1190
0.1517
0.1770
0.2022
0.7377

0.0000
0.0000
0.0000
0.0067
0.1530
0.2698
0.4102
0.5583
0.7293
2.1273

E(t)/
0.0000
0.0000
0.0000
0.0100
0.2932
0.6423
1.1683
1.8553
2.7696
6.7387

GRAPH 3

GRAPH 4

8.0

CALCULATIONS
SAMPLE CALCULATION
Experiment 1:

Area = (0.00.0) + (1.70.5) + (1.80.5) + (1.80.5) + (1.70.5) + (0.70.5) + (0.20.5)

+ (0.00.5) + (0.00.5)
= 3.95
For t=0.5;

RESIDENCE TIME DISTRIBUTION (RTD) FUNCTION FOR PLUG FLOW REACTOR

Experiment 1:
For time ( 0.0 -0.5 ) minutes

Area = (

= (0.5-0.0)

= 0.0538

= (1.0-0.5)

= 0.1108

= (1.5-1.0)

= 0.1139

= (2.0-1.5)

= 0.1108

For time ( 0.5-1.0 ) minutes

Area = (
For time ( 1.0-1.5 ) minutes

Area = (
For time ( 1.5-2.0 ) minutes

Area = (
For time ( 2.0-2.5 ) minutes

Area = (

= (2.5-2.0)

For time ( 2.5-3.0 ) minutes

Area = (

= (3.0-2.5)

= 0.0285

For time ( 3.0-3.5 ) minutes

Area = (

= (3.0-2.5)

= 0.0063

= (3.0-2.5)

= 0.0000

For time ( 3.5-4.0 ) minutes

Area = (

= Total area under the graph = (0.0538 + 0.1108 + 0.1139 + 0.1108 + 0.0760 +
0.0285 + 0.0063) = 0.5001

= 4(0.5001) = 2.0004

Second moment, variance,

E(t) dt

= 0.5643

Third moment, skewness,

E(t) dt
= 1.0824

9.0

DISCUSSION

The experiment was conducted to examine the effect of a pulse input and step change in a
tubular reactor and 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 constant
flowrate 700 mL/min for both experiment 1 and 2. While the experiment is running, the
conductivity for the inlet and outlet of the solution had been recorded at the period of
time at intervals of 30 seconds until the conductivity of the solution is constant.
For this experiment, we are examined the effects of flow for two types of reaction which
are in pulse input and step change. In this experiments, the graph of outlet conductivity
versus times had been plotted for both experiment. Based on graph of pulse input, the
outlet conductivity increase from 0.0 mS/cm at 0 minute to the highest value of 1.8
mS/cm at time of 1.0 minutes. After that, its value is contant at 1.8 mS/cm for 1.5 minute
before decrease within the time and comes to reach 0.0 mS/cm at the time of 3.5 minutes.
From the result, it showed that the result was not differ from the theory which shown that
the conductivity is reaching zero at time of 4 minutes.
In the other hand, for the graph of step change the outlet conductivity is increase within
the time by started at time 1.5 minutes which it outlet conductivity is 0.1 mS/min and
then undergoes some increament until at minutes 3.0 which the outlet conductivity is 1.7
mS/min. From there to minute 4.0, the value is contant at 1.7 mS/cm. From this two
graphs of step change and pulse input, we can see that 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.
Next experiment, to construct the residence time distribution (RTD) function for the
tubular flow reactor for pulse input and also step change. 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 almost same with the graph that are stated at the theory.
From the graph, it can be concluded tha the residence time distribution is depends on the
outlet conductivity.
For the pulse input graph, the residence time distribution calculated is 2.0004 minutes.
There are also 3 other datas that had been obtained and calculated which are mean
residence time,

tm ,

variance (second moment),2 and skewness (third moment),s 3 that

recorded 0.3557, 0.5643 and 1.0824 respectively. The skewness for the pulse input give a
positive value and so it called as a positive skew.
Compare ot the step change, the graph 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 distribution that calculated is 0.7377 minutes. The other
2 data are also need to be calculate which are variance (second moment), 2 and skewness
(third moment), s3 are 2.1273 and 6.7387 respectively. The skewness give a positive
value and it called positive skew.

10.0

CONCLUSION

From the experiment, we are able to examine the effect of the pulse input and step change
in a tubular flow reactor by differentiating both of the effect. Besides, we were also able
to construct the residence time distribution (RTD) function for the tubular flow reactor.
The conductivity for inlet and outlet after 4 minutes for pulse input are both 0.00 mS/min
while for the step change is 2.6 mS/min and 1.7 mS/min respectively. The outlet
conductivity, C(t) that had been calculated for pulse input is 3.95 and for step change is
4.1. The distribution of exit time, E(t) is calculated for each 30 second until 4 minutes
interval. The sum of E(t) for pulse input and step change are both 0.9999. The mean
residence time, tm for pulse input is 0.3557 minutes and step change is 0.7377 minutes.
The variance, 2 and skewness, s3 for pulse input are 0.5643 and 1.0824 while for step
change are 2.1273 and 6.7387. Graph for outlet conductivity, C(t) against time and
distribution of exit time, E(t) against time are plotted. The graph plotted almost the same
as the theory which stated that exit time, E(t) is depends on the value of C(t).

11.0

RECOMMENDATIONS

i.

The flow rate of fluid in the reactor must constant at 700 mL/min all the time
during the experiment. This is because the flow rate is always reset when we
switch on and off the pump.

ii.

All the flow valves need to be examine and testing need to be done before the
experiment is carried out so that all the data needed for the experiment can be
obtained.

iii.

Make sure that only one person doing the reading. This is due to the fluctuation of
the inlet and outlet conductivity reading panel.

iv.

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.

v.

And also make sure in the storage tank is always with a solution and not it will be
empty. It will cause error the whole experiment when it carried out.

vi.

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.

vii.

Make sure there are no leakages at the equipment.

12.0

REFERENCES

i.

Lab Manual Lab 6 ( Tubular Flow Reactor ) by Faculty of Chemical Engineering

UiTM Shah Alam

ii.

Fogler, H.S (2006). Elements of Chemical Reaction Engineering, 4th Edition,

New Jersey:Prentice Hall

iii.

http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm < 15 April

2015 >

iv.

http://encyclopedia.che.engin.umich.edu/Pages/Reactors/PFR/PFR.html
April 2015 >

<

16

13.0

APPENDIX