CHEMICAL REACTION ENGINEERING LAB

BKF3741

2019/2020 SEMESTER 2

TITLE OF EXPERIMENT: RESIDENCE TIME DISTRIBUTION ANALYSIS OF A

CONTINUOUS STIRRED TANK REACTOR

DATE OF EXPERIMENT: 10 MARCH 2020

INSTRUCTOR’S NAME: DR SHARIZA BINTI JAMEK

GROUP MEMBER:

NO NAME ID
.
1 SHAMALAH A/P SIVEM KA17010
2 NOR AZRI SYAZANA BINTI MOHD SABRI KA17054

3 NURUL AIN ATHIRAH BINTI AHMAD ZAIDI KA17174

4 KONG YEW BEN KA17197
5 MUHAMMAD NAJMI AMIR BIN AB RAZAK KA17293
6 DEEVIYE DARSHNI SRITHRAN KA17062

GROUP: 02

SECTION: 02

1
1.0 ABSTRACT

The objectives of this experiment are to obtain Residence Time Distribution data from tracer
injection in CSTR salts and to estimate the Residence Time Distribution.
The experiment started by preparing the calibration curve for conversion vs
conductivity. A calibration curve is done by preparing a series of different salt concentration
by dilution with deionized water. The conductivity is being measured and recorded according
to the series of different salt concentration that is diluted. For the next part of experiment,
mixture of 1500mL deionized water with 5 g salt and 5L of deionized water were prepared.
5L of deionized water is poured into tank 2 and the flow rate is adjusted to 150 mL/min. The
pump was switched on. After several minutes, some of deionized water will filled in the
CSTR (CT3) then the mixture of 1500mL and 5g salt solution was transferred into it. The
stirrer was started and kept at 200 rpm speed. The conductivity readings were recorded at
every 2minute interval until constant value reached. Liquid from the reactor is drained and
flushed once experiment ends and all apparatus are cleaned thoroughly. From Figure 1, the
concentration increases linearly with conductivity reading. This is due to the higher
concentrations of ions such as natrium ions, will contribute to greater the conductivity
reading as well as conversion. From the graph concentration vs time in Figure 3, the peak is
at 0.0576 and the value is decreasing until it reached constant which is -0.0005. Meanwhile,
Figure 4 show the graph of RTD against time which shows the peak is at 0.1184 and then the
value decrease until reaching constant rate of -0.0010. Hence, the value of concentration and
E(t) are decreasing with the time. This is due to the reactant is well mixed in the reactor.

2
 2.0 INTRODUCTION

In chemical engineering and related fields, the residence time distribution (RTD) is
defined as the probability distribution of time that solid or fluid materials stay inside one or more
unit operation in a continuous flow system. In an ideal CSTR the concentration of any substance
in the effluent stream is identical to the concentration throughout the reactor. Consequently, it is
possible to obtain the RTD from conceptual considerations in a fairly straight forward manner.
But as we know that no reactor in the world is ideal and hence all the atoms or molecules
entering the reactor don’t spend the same amount of time. To measure the non-ideality in a
reactor we plot a residence time distribution of atoms in the reactor. To define it, RTD of
a reactor is a characteristic of the mixing that occurs in the chemical reactor. Non ideal comes
into the picture and due to some disturbances in mixing the concentration of the exit effluents is
not the same as that is there in the reactor. Experimentally, RTD is determined by injecting a
tracer (which is normally an inert substance) in the reactor at some time t = 0 and then by
measuring the tracer concentration in the effluent stream as a function of time. Some typical
characteristics of a tracer are :

 The tracer used should be a nonreactive species that is easily detachable.

 Should have similar physical properties to those of the reacting mixture and be
completely soluble in the mixture. This is required so that the tracer’s behaviour will
honestly reflect that of the material flowing
 It should not adsorb on the walls or other surfaces in the reactor
The outlet concentration is then measured as a function of time. Material balance on an inert
tracer that has been injected as a pulse at time t = 0 into a CSTR for t >0

Integrating the above the above equation with C = Co at t = 0, we geT

We would further take C (t) as the measure of concentration of tracer as a function of time.

3
3.0 METHODOLOGY

A series of different salt concentrations (NaCl) was

prepared by dilution with deionized water.
The conductivity value was obtained from the
conductivity meter
Preparation Of
Calibration Curve

The tank was topped up with water.

The valve below the CSTR tank was closed.
The CSTR tank was filled up with water until it
overflowed.
The volume of the water in the CSTR tank at overflow
condition was about 1500 mL.
5.0g of salt was transferred into the CSTR tank.
The stirrer was started and stirred at a speed of 200 rpm.
Experimental The conductivity meter was continuously monitered until
Procedure it reached constant value.
The flow was adjusted to 150 mL/min and the timer was
started after the flow pump was turned on.
The conductivity reading was obtained at every 2
minutes interval for at least 30 minutes.

Any liquids were drained off from the reactor and the
reactor was made sure that it was cleaned properly after
the experiment was completed.
All liquids were disposed immediately after each
experiment.
Shutdown The reactor was flushed with water 2 times.
Procedure
4
4.0 RESULTS

1.5 L distilled water used to dissolve sodium chloride (NaCl) in different mass and different
concentration is obtained.
Concentration of NaCl solution is calculated using the formula below:
mol mass( g)
Concentration( )=
l g
molecular weight( )× volume (l)
mol
Molecular weight for NaCl = 58.44 g/mol

Calibration Curve

Weight (g) Conductivity (mS/cm) Concentration (mol/L)

0.5 0.73 0.0057
1.0 1.37 0.0114
1.5 2.00 0.0171
2.0 2.61 0.0228
2.5 3.22 0.0285
3.0 3.83 0.0342
3.5 4.45 0.0399
4.0 5.04 0.0456
4.5 5.68 0.0513
5.0 6.28 0.0570
Table 1: Conductivity reading with different concentrations of NaCl solution.

Flow rate: 150 mL/min

Time (min) Conductivity (mS/cm)

5
0 6.35
2 4.88
4 4.31
6 3.50
8 2.76
10 2.18
12 1.74
14 1.40
16 1.10
18 0.88
20 0.70
22 0.56
24 0.45
26 0.36
28 0.30
30 0.24
32 0.20
34 0.17
36 0.14
38 0.12
40 0.10
42 0.08
44 0.08
46 0.08
Table 2: Conductivity reading with respect to time

6
 Calibration Curve
7
6 f(x) = 107.87 x + 0.14
R² = 1
5
Conductivity (mS/cm)

4
3
2
1
0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration (mol/L)

Figure 1: Graph of conductivity against concentration

Conductivity vs time
7
6
Conductivity (mS/cm)

5
4
f(x) = − 0.11 x + 3.8
3 R² = 0.73

2
1
0
0 5 10 15 20 25 30 35 40 45 50
Time (min)

Figure 2: Graph of conductivity against time

7
5.0 DISCUSSION

Calibration Curve
7
6 f(x) = 107.87 x + 0.14
R² = 1
5
Conductivity (mS/cm)

4
3
2
1
0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration (mol/L)

Figure 3: Graph of conductivity against concentration

Based on Figure 1, the relationship between concentration and conductivity can be related with
an equation:
y = 107.87x + 0.1393

8
 Conductivity vs time
7
6
Conductivity (mS/cm)

5
4
f(x) = − 0.11 x + 3.8
3 R² = 0.73

2
1
0
0 5 10 15 20 25 30 35 40 45 50
Time (min)

Figure 2: Graph of conductivity against time

Based on figure 2, the graph of conductivity against time shows that conductivity decreases
exponentially with time.
The concentration can be determined based on the equation obtained from the calibration curve
as shown below:
y = 107.87x + 0.1393

Time (min) Conductivity Concentration RTD Function,

(mS/cm) (mol/L) E(t)
0 6.35 0.0576 0.1184
2 4.88 0.0439 0.0903
4 4.31 0.0387 0.0796
6 3.50 0.0312 0.0641
8 2.76 0.0243 0.0500
10 2.18 0.0189 0.0389
12 1.74 0.0148 0.0304
14 1.40 0.0117 0.0241
16 1.10 0.0089 0.0183
18 0.88 0.0069 0.0142
20 0.70 0.0052 0.0107
22 0.56 0.0039 0.0080

9
 24 0.45 0.0029 0.0060
26 0.36 0.0020 0.0041
28 0.30 0.0015 0.0031
30 0.24 0.0009 0.0019
32 0.20 0.0006 0.0012
34 0.17 0.0003 0.0006
36 0.14 0.0000 0.0000
38 0.12 -0.0002 -0.0004
40 0.10 -0.0004 -0.0008
42 0.08 -0.0005 -0.0010
44 0.08 -0.0005 -0.0010
46 0.08 -0.0005 -0.0010
Table 3: Concentration of salt solution and residence time distribution function data for
each time

From the concentration obtained, the value of residence time distribution (RTD) function, E (t)
can be calculated by using the equation below [ CITATION Fog11 \l 1033 ];
C(t )
E ( t )= ∞
∫ C ( t ) dt
0

∞
The value of ∫ C ( t ) dt can be calculated using Simpson’s rule. The formula for Simpson’s rule is
0

given below [ CITATION Dal05 \l 1033 ]:

Simpson’s three eighths rule (four-point):
X3
3
∫ f ( X ) dX= 8 h[ f ( X 0 ) +3 f ( X 1 ) +3 f ( X 2 ) + f ( X 3 ) ]
X0

X 3−X 0
where h= X 1 =X 0 +h X 2 =X 0 +2 h
3

From 0 minute until 42 minutes, Simpson’s three-eighths rule can be used whereby it requires
four points. The calculations for Simpson’s rule are shown below:

∫ C ( t ) dt = 38 (2)[ ( 0.0576 ) +3 ( 0.0439 ) +3 ( 0.0387 )+ ( 0.0312 )]=0.2525

0

10
12

∫ C ( t ) dt = 38 (2)[ ( 0.0312 ) +3 ( 0.0243 ) +3 ( 0.0189 ) + ( 0.0148 ) ]=0.1317

6

18

∫ C ( t ) dt= 38 (2)[ ( 0.0148 ) +3 ( 0.0117 ) +3 ( 0.0089 ) +( 0.0069 ) ]=0.0626

12

24

∫ C ( t ) dt = 38 (2)[ ( 0.0069 ) +3 ( 0.0052 ) +3 ( 0.0039 ) + ( 0.0029 ) ]=0.0278

18

30

∫ C ( t ) dt= 38 (2)[ ( 0.0029 ) +3 ( 0.0020 ) +3 ( 0.0015 ) +( 0.0009 ) ]=0.0108

24

36

∫ C ( t ) dt = 38 (2)[ ( 0.0009 ) +3 ( 0.0006 ) +3 ( 0.0003 ) + ( 0.0000 ) ]=0.0026

30

42

∫ C ( t ) dt= 38 (2)[ ( 0.0000 ) +3 (−0.0002 ) +3 (−0.0004 )+ (−0.0005 ) ]=−0.0016

36

Simpson’s one-third rule (three-point):

X2
h
∫ f ( X ) dX= 3 [f ( X 0 ) +4 f ( X 1 ) + f ( X 2 ) ]
X0

X 2−X 0
where h= X 1 =X 0 +h
2
From 42 minutes until 46 minutes, Simpson’s one-third rule can be used whereby it requires four
points. The calculations for Simpson’s rule are shown below:
46

∫ C ( t ) dt= 23 [ (−0.0005 ) + 4 (−0.0005 ) +(−0.0005 ) ]=−0.0022

42

46

∫ C ( t ) d=¿ 0.2525+ 0.1317+0.0626+0.0278+ 0.0108+ 0.0026+ (−0.0016 )=0.4864 ¿

0

Thus, to calculate E(t), we can use the equation below:

C( t)
E ( t )=
0.4864

11
 Graph of concentration vs time
0.07
0.06
Concentration (mol/L)

0.05
0.04
0.03 f(x) = − 0 x + 0.03
R² = 0.72
0.02
0.01
0
0 5 10 15 20 25 30 35 40 45 50
-0.01
Time (min)

Figure 3: Graph of concentration against time

From Figure 3, we can observe that the concentration decreases with time. The longer the
time, the lower the concentration obtained. To obtain E(t) curve, we simply divide the C(t) with

the area under the curve represented by the integral,∫ C ( t ) dt.

0

Graph of RTD Function,E(t) vs time

0.1400
0.1200
0.1000
RTD Function,E(t)

0.0800
0.0600 f(x) = − 0 x + 0.07
0.0400 R² = 0.72
0.0200
0.0000
0 5 10 15 20 25 30 35 40 45 50
-0.0200
Time(min)

Figure 4: Graph of RTD Function against time

12
 Based on Figure 4, we can observe that the E(t) decreases with the time. According to the
study, the graph should produce a narrow peak and moves closer to unity afterwards if it is an
ideal CSTR. Based on the graph that we obtained, it shows a narrow peak, so we can assume it is
an ideal CSTR. The ideal condition means the reactant is well mixed in the reactor and there is
no dead volume present in the reactor. In an ideal single CSTR, the concentration of any
substance in the effluent stream is identical to the concentration throughout the reactor.
Moreover, an ideal CSTR has complete back-mixing resulting in a minimisation of substrate
concentration and maximisation of the product concentration, relative to the final conversion at
every point within the reactor the effectiveness factor being uniform throughout. Commonly,
RTD is used to diagnose problems in existing reactors. Figure 4 illustrates the RTDs resulting
from the experimental data, showing that the CSTR reactor operate at nearly ideal condition
which means near perfectly mixing of reactant in the CSTR.

13
6.0 CONCLUSION & RECOMMENDATION

In conclusion, NaCl solution shown increased in conductivity as mass of NaCl which

proposed that mass of NaCl is directly proportional towards conductivity. However, if mass of
NaCl is constant and being run over a CSTR using water to dilute the solution, it is decreasing in
an exponential rate until it reaches a constant value of 0.08 mS/cm after 46 minutes which
indicate the reactor is entering steady state of the mixing process. The exponential graph also
shows that the reactor is not performing in an ideal condition.
For recommendation, we suggest that to avoid error and minimise the standard deviation
of conductivity reading, the conductivity meter should be rinsed with distilled water after every
reading to avoid any contamination towards the next reading. In addition, the reactor should be
rinsed with distilled water to wash off any salt or remnants left behind by previous
experimentation. A trial of experiment is supposed to be done before conducting the experiment
by using distilled water to allow preparation such as adjusting rotational speed of the mixer and
the flow rate of the water into the reactor. Lastly, the water level has to be consistently monitored
and added in before it reaches ¼ of the tank to allow sufficient time for water to continuously
flow into the reactor without any disturbance.

14
7.0 REFERENCE

I. Fogler, H Scott (2011). Elements of Chemical Reaction Engineering, Upper Saddle

River, N.J. :Prentice Hall PTR
II. Gao et al (2012). A Review Of The Residence Time Distribution (RTD) Applications In
Solid Unit Operations

15