1.

0 ABSTRACT

The objectives of the experiment of residence time distribution analysis of a continuous stirred tank
reactor were to obtain RTD data from tracer injection and to estimate RTD parameters. The
experiment was started with the preparation of calibration curve for the concentration of table salt
(NaCl) versus conductivity by manipulating the mass of NaCl from 1 g, 2 g, 3 g, 4 g and 5 g in 1500 mL
deionized water respectively to obtain the conductivity for different concentration of NaCl. For the
second part, all the apparatus and reactors were set up according to the experimental procedure and
only CT3 were used for the RTD study. Tank 2 (T2) was filled up with 1500 mL deionized water and 5
g of table salt was transferred into T2. The stirring process was started at speed of 200 rpm.
Conductivity meter was continuously monitored until it reached a constant value. Rotameter V2 was
turned on and the flow was adjusted to 150 mL/min. The conductivity reading was determined at
every 2 minutes interval until the reading of conductivity became constant. All the observation was
recorded. Based on the calibration curve, the concentration of NaCl was directly proportional to its
conductivity due to the ionization of NaCl producing free moving ions in the compound. The
performance of CSTR in the second experiment depend on the flow and mixing patterns in the reactor
to a great extent. As time progress, the conductivity of NaCl decreased due to the decreased in
concentration of sodium chloride ions in CSTR ad dilution occurred. Besides, the residence time
distribution function, E(t) decreased as time increased. Hence it could be concluded that the reactor
behaved as an ideal CSTR and it operated without bypassing with a dead volume but slightly dead
zone.

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 2.0 METHODOLOGY

1.1 Preparation of calibration curve

The steps were

1 g NaCl was The conductivity of repeated by
weighed and the solution was using 2 g, 3 g, 4
mixed with obtained using g and 5 g of
1500 mL of conductivity meter NaCl
water. and tabulated.

1.2 Experimental procedure

The pump was started and

CSTR experimental The tank was top up rotameter was adjusted to
vessel was set up with water. the maximum reading to
fill up the reactor until it
overflows. The volume of
the reactor at overflow
condition about 1500 mL.

The conductivity meter

was continuously 5.0 g of table salt was
monitored until transferred into the reactor.
constant value had The stirrer was started and The pump was turned off
reached. the stirring speed was kept upon attained a steady
at 200 psi. flow.

Rotameter was turned on The conductivity reading

and the flow was adjusted to was obtained at every 2
150 mL/min and the timer minutes interval for at least
was started 30 minutes.

1.3 Shutdown procedure

Any spillage from the unit was
Any liquids from the reactor All liquids were
wiped off immediately. The
were drained off and cleaned immediately reactor was flushed with water
properly. disposed after for 2 times.
each experiment.

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3.0 RESULT & DISCUSSION
3.1 Calculations and Results

Preparation of Calibration Curve

By increasing 1 g mass of NaCl is dissolved in 1.5 L of distilled water for each sample will give the
different concentration of NaCl solution. The concentration of NaCl solution can be calculated by:

𝑚𝑜𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑁𝑎𝐶𝑙(𝑔)

𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 ( )= 𝑔
𝐿 𝑀𝑊 ( ) × 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝐿)
𝑚𝑜𝑙

Molecular weight NaCl = 58.44 g/mol

Volume of solution = 1.5 L

Mass of table salt (g) Concentration of NaCl Conductivity (mS/cm)

solution (mol/L)
0 0.0000 0.04

1 0.01141 1.54

2 0.02282 2.92

3 0.03422 4.27

4 0.04563 5.57

5 0.05704 6.76

Table 1: Conductivity against Concentration

3
 Conductivity against Concentration
8

7
y = 117.82x + 0.1567
6 R² = 0.9987
Conductivity (mS/cm)

0
0.00000 0.01000 0.02000 0.03000 0.04000 0.05000 0.06000
Concentration (mol/L)

Graph 1 Conductivity against Concentration

Based on the Graph 1, the relationship between conductivity and concentration:

𝑦 = 117.82𝑥 + 0.1567

Where y is conductivity and x is concentration.

Therefore, equation of concentration function of conductivity is

𝑦 − 0.1567
𝑥=
117.82

This equation use to determine experimental concentration from recorded conductivity.

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Experimental result

Time (min) Conductivity Concentration (mol/L)

(mS/cm)

0 5.46 0.04501
2 4.58 0.03754
4 3.52 0.02855
6 2.79 0.02235
8 2.24 0.01768
10 1.75 0.01352
12 1.32 0.00987
14 1.05 0.00758
16 0.84 0.00580
18 0.63 0.00402
20 0.53 0.00317
22 0.40 0.00207
24 0.32 0.00139
26 0.26 0.00088
28 0.20 0.00037
30 0.17 0.00011
32 0.14 -0.00014
34 0.12 -0.00031
36 0.10 -0.00048
38 0.08 -0.00065
40 0.07 -0.00074
42 0.07 -0.00074
44 0.07 -0.00074
Table 2: Conductivity and concentration for every 2 minutes

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3.2 Discussion
1. Plot the transient concentration profile.

Concentration against Time

0.05000

0.04000
Concentration (mol/L)

0.03000

0.02000

0.01000

0.00000
0 5 10 15 20 25 30 35 40 45 50
-0.01000
Time (min)

Graph 2: Transient concentration profile

Graph 2 shown, the concentration of the NaCl is decreasing when the time increase. The decreasing
concentration of NaCl in CSTR because of dilution happened.

2. Determine the RTD parameters based on the collected data.

From Fogler (2006), Appendix A.4 can be used to find the area under Graph 2.

By using Simpson’s rule:

For N +1 points, where N is even,

𝑋𝑁 ℎ
∫ 𝑓 ( 𝑋 ) 𝑑𝑋 = ( f0 + 4 f1 + 2 f2 + 4 f3 + 2 f4 + … + 4 fN -1 + fN )
𝑋0 3

𝑋𝑁 −𝑋0
where ℎ = 𝑁

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Area under the graph in Graph 2 can be determine by Simpson’s rule above since graph contains
22+1 points, where 22 is even.

44
∫0 𝐶(𝑡) = 0.04501 + 4(0.03754) + 2(0.02855) + 4(0.02235) + 2(0.01768) +
4(0.01352) + 2(0.00987) + 4(0.00758) + 2(0.00580) + 4(0.00402) +
2(0.00317) + 4(0.00207) + 2(0.00139) + 4(0.00088) + 2(0.00037) +
4(0.00011) + 2(−0.00014) + 4(−0.00031) + 2(−0.00048) + 4(−0.00065) +
2(−0.00074) + 4(−0.00074) + (−0.00074)

44
∫0 𝐶(𝑡) = 0.34713 𝑚𝑜𝑙. 𝑚𝑖𝑛/𝐿

E(t) can be found by using the following formula:

𝐶(𝑡) 𝐶(𝑡)
𝐸(𝑡) = 44 =
∫0 𝐶(𝑡) 0.34713

Time (min) Mean Conductivity Concentration (mol/L) E(t) (min-1)

(mS/cm)
0 5.46000 0.04501 0.12967
2 4.58000 0.03754 0.10815
4 3.52000 0.02855 0.08224
6 2.79000 0.02235 0.06439
8 2.24000 0.01768 0.05094
10 1.75000 0.01352 0.03896
12 1.32000 0.00987 0.02844
14 1.05000 0.00758 0.02184
16 0.84000 0.00580 0.01671
18 0.63000 0.00402 0.01157
20 0.53000 0.00317 0.00913
22 0.40000 0.00207 0.00595
24 0.32000 0.00139 0.00399
26 0.26000 0.00088 0.00253
28 0.20000 0.00037 0.00106
30 0.17000 0.00011 0.00033
32 0.14000 -0.00014 -0.00041
34 0.12000 -0.00031 -0.00090
36 0.10000 -0.00048 -0.00139
38 0.08000 -0.00065 -0.00188
40 0.07000 -0.00074 -0.00212
42 0.07000 -0.00074 -0.00212

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 44 0.07000 -0.00074 -0.00212
Table 3: Residence time distribution data

E(t) against Time)

0.14000

0.12000

0.10000

0.08000
E(t) (min-1)

0.06000

0.04000

0.02000

0.00000
0 5 10 15 20 25 30 35 40 45 50
-0.02000
Time (min)

Graph 3: Residence time distribution

Based on Graph 3, the residence time distribution function, E(t) is decreasing as the time increase.

3. From the trend of RTD, suggest prevailing issues. Determine whether the reactor is an ideal CSTR?
The residence time is the time for a fluid to stay in the reactor once entering. Residence time
distribution (RTD) is a useful diagnostic tool to characterize the mixing and flow within reactors and
to compare the behavior of real reactors to their ideal models. Feed introduced into a CSTR at any
given time becomes completely mixed with the material already in the reactor. In other words, some
of the atoms entering the CSTR leave it almost immediately because material is being continuously
withdrawn from the reactor; other atoms remain in the reactor almost forever because all the
material is never removed from the reactor at one time. Many of the atoms, of course, leave the
reactor after spending a period of time somewhere in the vicinity of the mean residence time.

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Figure 1: Perfect operation of a CSTR (Fogler, 2006)

From Graph 3 that the typical RTDs resulting from the CSTR shows that it is near perfectly mixed
CSTR and have a slightly dead zone in which the tracer slowly diffuses in and out. Death zone is a
region where there is little or no exchange of material with the well-mixed region, and, consequently,
virtually no reaction occurs there. Moreover, the CSTR used in this experiment operates without
bypassing but is with a dead volume. Figure 1 shows the behavior of a perfect operation of an ideal
CSTR, which illustrates the typical RTDs resulting from an ideal CSTR.

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4.0 CONCLUSION & RECOMMENDATION

In conclusion, the experiment was conducted and the effect of residence time distribution on
CSTR was observed. The objectives are achieved where are RTD is obtained from tracer injection and
RTD parameters are recorded. From the reading of CSTR, a series of conductivity value is observed
from the screen which is decreased as the time increased. As calculated, the concentration of NaCl is
decreasing with time. The plotted graph of concentration of NaCl versus time showing that
concentration of NaCl is inversely proportional to the time. Based on the value obtained from the
experiment, the residence time distribution function is calculated and the graph plotted is inversely
proportional due to the residence time distribution function decreasing as the time increase. In
addition, the residence time distribution graph presents the condition of CSTR in which it operates
nearly in an ideal condition where it operates without bypassing with a dead volume but slightly dead
zone.
In the experiment, there must be some errors when handling the chemical reactant or operating
the reactor. There are some suggestions to reduce the error to get an accurate result. Based on the
graph of residence time distribution function versus time, it is clearly showed that there is dead
volume present in the reactor. When a dead volume is present, a decreased amount of material is
observed in the output stream. Firstly, the stream flow should be visually examined with transparent
fluid like water or air and a small amount of color tracer injection of traces should be placed in the
tube which delivers mainstream and after the injection tube there should be kenics static mixer or
similar device to evenly distribute tracer in the whole volume of the stream. Next, inlet and outlet
tube in the reactor should be placed as far as possible apart. Besides, the conductivity meter must be
ensured is well calibrated before used to reduce the instrumentation error. For instance, the
conductivity meter must also be rinsed with the water after taking each reading. In addition, the
reactor must first be purged with the pure water to remove and flash out the impurity which might
alter the conductivity reading. Lastly, the flow rate must be kept constant throughout the experiment
by adjusting the value of the flow rate.

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5.0 REFERENCE

Fogler, H.S. (2006). Distributions of Residence Times for Chemical Reactor. In H.S. Fogler, Elements
Of Chemical Reaction Engineering (p. 868-894). Pearson Education, Inc.

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