UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY 3
CHE (574)
NAME
: NIK NUR SHAHIRA BINTI IBRAHIM (2012209148)
GROUP
: EH220(4A)
EXPERIMENT
: EXPERIMENT OF TUBULAR FLOW REACTOR BP 101B
DATE PERFORMED : 9 APRIL 2014
SEMESTER
:4
PROGRAMME / CODE : CHE 574
SUBMIT TO
: DR JEFRI JAAPAR

No.
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Title
Abstract/ Summary
Introduction
Aims
Theory
Apparatus
Methodology/ Procedure
Result
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix

TOTAL MARKS
Remarks:
Checked by:
_________________
Date:

Allocated Marks
(%)
5
5
5
5
5
10
10
20
20
10
5
5
5
100

Marks

Contents
Abstract........................................................................................................................ 3
Introduction.................................................................................................................... 3
Aims............................................................................................................................ 3
Theory.......................................................................................................................... 4
Apparatus...................................................................................................................... 5
Procedure...................................................................................................................... 8
Result......................................................................................................................... 10
Discussion................................................................................................................... 10
Conclusion................................................................................................................... 17
Recommendations.......................................................................................................... 18
Reference.................................................................................................................... 18
Appendix..................................................................................................................... 19

Abstract
Reactors are widely used in the chemical industrys processes. One of type of reactors is
tubular reactor. The flow in tubular flow reactor is continuous and in a steady state condition and
configured so that conversion of the chemicals and other dependent variables are functions
of position within the reactor. A unit called SOLTEQ Tubular Flow Reactor (Model: BP 101-b) is
used in this experiment. This experiment is divided into two which are to examine the effect of
pulse input in a tubular flow reactor and the other is to examine the effect of step change input in
a tubular flow reactor. Besides that, to compare the residence time distribution (RTD) graph
between these two experiments. The mean residence time, variance, and skewness are also
calculated for both experiments.

Introduction
Chemical reactor is a place where chemical reactions take place and it is one of the
important part of any chemical process design. 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 are likely as the batch reactors in providing initially
high driving forces. Flow in tubular reactors can be laminar with viscous fluids in small diameter
tubes and greatly deviate from ideal plug flow behavior; or turbulent as with gases. Establishing
turbulent flow can result in inconveniently long reactors or may require unacceptably high feed
rates for slow reactions and especially in small laboratory and pilot plant reactors. The design of
systems with tubular reactors involves recognition of the many important differences between
continuous stirred tank reactors (CSTR) and plug flow tubular reactors (PFR).The most important
distinction is the importance of the feed conditions in tubular reactor systems, particularly the
reactor inlet temperature. Reactor feed preheating becomes an important design parameter, which
typically involves trades off between steady state economics and dynamic controllability.
Reactor inlet concentrations are also more critical in tubular reactor systems, because of
parametric sensitivity and the potential for complex dynamics.

Aims

Experiment 1

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

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

Experiment 2

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

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

Theory
Residence time distribution (RTD) Function
The residence time distribution (RTD) of a reactor is a characteristic of the mixing that
occurs in the chemical reactor. No axial mixing in a plug flow reactor (PFR). The continuous
stirred tank reactor (CSTR) is thoroughly mixed. Actually, different reactors can display identical
RTD. However, the RTD exhibited by a given reactor yields distinctive clues to the type
of mixing. The RTD is determined by experimentally by injecting an inert chemical called a
tracer into the reactor at some time t = 0 and measuring the tracer concentration, C in the effluent
stream as a function time. There are two types method of injection which are pulse input and step
input.

Pulse Input
An amount of tracer

N0

is suddenly injected in one shot into the feed stream entering

the reactor in as short time as possible in pulse input. The outlet concentration is then measured
as a function of time. The effluent concentration vs. time curve is referred to as the C(t) curve in
the RTD analysis. The amount of tracer C(t) exiting between time t and (t + t) is

(t) vt

Where v = the effluent volumetric flow rate

If it divided by the total amount of material that was injected into the reactor,
N vC (t)
=
N0
N0

N0

which represents the fraction of material that has residence time in the reactor between time t and
(t + t).

For a pulse injection,

E (t)=

vC( t)
N0

N
=E ( t )
N0

1
t

E (t) called as the residence time distribution function. It is describes how much time different
fluid elements have spent in the reactor.
It can be obtained from the outlet concentration measurements by summing up all the
N0
amounts of materials if
is not known directly. N between time t=0 and infinity.
d

(t) vdt

By integrating,

N 0= vC ( t ) dt
0

By assuming v is constant, substitute 2 into 1

E (t)=

C (t)

C ( t ) dt
0

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

Step Input
A more general relationship can be developed between a time-varying tracer injection and
the corresponding concentration in the effluent by understanding the pulse input. The below
show the output concentration from the vessel is related to the input concentration by the
convolution integral,

By considering a constant rate of tracer addition to a feed in order to analyze a step input
in the tracer concentration with constant volumetric flow rate that is initiated at time t=0.

Because the inlet concentration is constant with time,

integral sign,

By dividing with

C0

yields,

The expression differentiated to obtain the RTD function E(t),

Formula for other calculation,

C0

, it can be taken outside the

Apparatus

Tubular flow reactor Model BP-101-B.

Sodium chloride solution, NaCl 0.025M.
Deionised water.

Procedure
General Start-up Procedure
1.
2.
3.
4.
5.

All valves were ensured initially closed except valve V7.

20 liter of salt solution was prepared. For example, sodium chloride, NaCl (0.025M).
The feed tank B2 was filled with the NaCl solution.
The power for the control panel was turned up.
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 700 ml/min at flow meter F1-01. The conductivity display
was observed at low value then a valve V10 was 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. Avalve V12 was closed and
pump P2 was switched off.
8. The unit was ready for experiment.
General Shutdown Procedures

1. Both pump P1, P2 and P3 were switched off. Valves V2 and V6 were 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 startup procedures are performed.
2. Valve V9 is opened and pump P1 is switched.
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 FI-01.
4. The deionized water is left to continue flowing through the reactor until the inlet(Q1-01)
and outlet (Q1-02) conductivity values are stable at lows levels. The both conductivity
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 stared 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 FI-02.
8. The salt solution is left to flow for 1 minute, and then the timer is reset and restarted. The
time is start at the average pulse input.
9. Valve V11 is closed and pump P2 is switch off. Then, quickly valve V9 is opened and pump P1 is
switch on.
10. The deionized water flow rate is making sure to always maintain at 700 mL/min by
adjusting the P1 flow controller.
11. Both the inlet (QI-01) and outlet (QI-02) conductivity values is recorded at regular
intervals of 30 seconds.
12. The conductivity values is continue recorded until all the readings are almost constant
and approach the stable low level values.
Experiment 2: Step Change Input in a Tubular Flow Reactor
1. The general startup procedures were 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 FI-01.
4. The deionized water is left to continue flowing through the reactor until the inlet (QI-01)
and the 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. 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 recorded until all readings are almost constant.

Result
Experiment 1:
Flow rate: 700 mL/min
Input type: Pulse Input
Time (min)
Inlet
0.0
0.1
0.0
0.0
0.0
0.0
0.0
0.0

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Time , min
0.0
Outlet
0.0
Conductivity,
mS/cm
E(t), 1/min
0.0000

Conductivity (mS/cm)
Outlet
0.0
2.1
2.2
2.2
2.1
1.0
0.3
0.0

0.5
2.1

1.0
2.2

1.5
2.2

2.0
2.1

2.5
1.0

3.0
0.3

3.5
0.0

0.4242

0.4444

0.4444

0.4242

0.2020

0.0606

0.0000

Outlet Conductivity vs Time

2.5
2
1.5
Outlet conductivity, mS/cm

1
0.5
0
0

0.5

1.5

2.5

3.5

Time, min

Figure 1: Outlet Conductivity vs Time

E(t) vs Time
0.5
0.45
0.4
0.35
0.3
E(t), 1/min

0.25
0.2
0.15
0.1
0.05
0
0

0.5

1.5

2.5

Time, min

Figure 2: RTD function plot, the E curve

3.5

Experiment 2:
Flow rate: 700 mL/min
Input type: Step Change Input
Time (min)
Inlet
0.0
2.9
3.2
3.3
3.3
3.3
3.3
3.3
3.4
3.3
3.3
3.3
3.3
3.3
3.3
3.3

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
Time , min
0.0
Outlet
0.0
Conductivity,
mS/cm
E(t), 1/min
0.0000

Time , min
Outlet
Conductivit
y, mS/cm
E(t), 1/min

Conductivity (mS/cm)
Outlet
0.0
0.0
0.0
0.0
0.0
0.1
1.4
1.8
1.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0

4.5
2.0

0.5
0.0

1.0
0.0

0.0000

0.0000 0.0000 0.0000 0.0104 0.1458 0.187

5

5.0
2.0

0.020 0.020
83
83

5.5
2.0

1.5
0.0

6.0
2.0

0.020 0.020
83
83

2.0
0.0

6.5
2.0

2.5
0.1

7.0
2.0

3.0
1.4

7.5
2.0

0.020 0.020 0.020

83
83
83

3.5
1.8

4.0
1.9

0.1979

Outlet Conductivity Vs Time

2.5
2
1.5
Outlet conductivity, mS/cm

1
0.5
0
0

Time, min

Figure 3: Outlet conductivity vs time

E(t) Vs Time
0.25
0.2
0.15
E(t), 1/min

0.1
0.05
0
0

Time, min

Figure 4: RTD function plot, the E curve

Calculations
Experiment 1
For outlet conductivity of 0.3 mS/cm:

Ci t

C ( t ) dt

0.5 min

C ( t ) dt
0

(0.3+2.1+1.0+2.2+2.2+2.1)

4.95

C ( t ) dt
0

C(t )
E (t) =

C ( t ) dt
0

E (t) =

0.3
4.95

E (t) =

0.0606

min1

Mean residence time

tm

t . E ( t ) dt

tm

0.5 0.0606
4.95

t E (t)
Ci t

(0.5)

tm

0.00612

Variance

(ttm ) E ( t ) dt
2

(t t m) E(t)
Ci t

(0.50.00612)2 (0.0606)
4.95

0.002986

Skewness
=

(t t m)3 E(t )
Ci t

s3

(0.50.00612) (0.0606)
4.95

s3

s3

1.47 x 10-3

Experiment 2
For outlet conductivity of 0.2 mS/cm:

Ci t

C ( t ) dt

0.5 min

(t t m)2 E(t)
Ci t

C ( t ) dt
0

(1.9+1.8+1.4+0.1+2.0+2.0+2.0+2.0+2.0+2.0+2.0) ( 0.5 )

9.6

C ( t ) dt
0

C(t )
E (t) =

C ( t ) dt
0

E (t) =
E (t) =

0.2
9.6
min

0.02083

Mean residence time

tm

t . E ( t ) dt

tm

0.5 0.02083
9.6

tm

1.085 x 10-3

t E (t)
Ci t

Variance

(ttm ) E ( t ) dt
2

(t t m)2 E(t)
Ci t

(t t m)2 E(t)
Ci t

3 2

(0.51.085 x 10 ) (0.02083)
9.6
5.40 x 10-4

Skewness
3

s3

(t t m) E(t )
Ci t
3 3

s3

(0.51.085 x 10 ) (0.02083)
=
9.6
=

2.69 x 10-4

Discussion
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.
There are two experiments for tubular reactor which are pulse input in a tubular reactor
and step change input in a tubular reactor. For first experiment, it was aimed to examine the

effect of a pulse input in a tubular reactor. Second experiment is to attain the effect of a step
input in a tubular reactor. From the result for these two experiments, the residence time
distribution (RTD) function which is E(t) as a function of time is plotted. From the both graph
that has been plotted, the trend for this two graphs are different. The trend for residence time
distribution (RTD) graph for first experiment for pulse input is increase and then for a few
minute is decreased until the value is zero. However, the graph for second experiment the graph
is increase and at time 2 min, the value of E(t) is constant. In these experiments, the mean residence time,
second moment (Variance), and third moment (Skewness) are also calculated. For experiment 1, the
mean residence time is 0.00612 min, second moment (variance) is 0.002986 min
third moment (Skewness) is 1.47 x 10-3 min

5 /2

and

for outlet conductivity of 0.3 mS/cm.

On the other hand, the mean residence time for experiment 2 is 1.085 x 10-3 min. Then, the
second moment (variance) is 5.40 x 10-4 min

and the third moment (Skewness) is 2.69 x

5 /2
10-4 min
.

This experiment shows that there are differences between pulse input and step change
input in tubular reactor method. One of the differences is the tracer of the input. In a pulse input,
an amount of tracer substance is suddenly injected in one shot into the feed stream entering the
reactor in as short times as possible. While for a step input, a constant rate of tracer addition to a
feed is initiated at time t = 0. Before this time no tracer was added to the feed. The tubular
reactor is usually used in some of the following application which is large scale reactions, fast
reactions, homogeneous or heterogeneous reactions, continuous production, and high
temperature reactions.

Conclusion
The objectives of these two experiments were achieved. As a conclusion, there are
differences for pulse input and step change input in a tubular reactor. The residence time
distribution (RTD) function is one of the differences for pulse input and step change input. For
RTD graph for pulse input experiment, the graph is increase and then decrease to the value

zero. However, the RTD graph for step change input, the graph is increase then constant
at certain value before decrease rapidly due to some error. Thus, the experiment was successful.

Recommendations
There are few suggestions to get more accurate results for this experiment, which are:

Ensure that no leakage at the valve on the unit. This to prevent the result will affect.
Make sure that the valve is open or close, follow as the general startup procedure

carefully.
For both experiments, do more trial to get average of conductivity for both inlet (Qi-01)
and outlet (QI-02) conductivity values in order to get more accurate results.

Reference
1. Fogler, H.S (2006). Elements of Chemical Reaction Engineering (3rd Edition). PrenticeHall.
2. Levenspiel, O. (1999). Chemical Reaction Engineering (3rd Edition). John Wiley.
3. Laboratory Manual Tubular Flow Reactor.

Appendix