Manipal University

Department of Chemical Engineering

CE 1732- Chemical Reaction Engineering Laboratory

IV YEAR, VIITH SEMESTER, 2018

EXPERIMENT #8
RTD Studies in a PFR

INSTRUCTORS:
Dr. Gaurav Bhaduri
Dr. Abhishek Sharma

GROUP #2
Akriti Agarwal - 159110003

Experiment carried on: October 12, 2018

Report submitted on: October 22, 2018

PRELAB (10) ______

EXECUTIVE SUMMARY (10) ______
INTRODUCTION/OBJECTIVES/SCOPE/PROCEDURE (30) ______
RESULTS & DISCUSSION (30) ______
a) Data analysis and interpretation of information
b) Presentation of relevant information (including results on graphical, tabular or equation
forms)
CONCLUSIONS (5) ______
REFERENCES (5) ______
APPENDIX
a) Original data, sample calculations, Excel sheets (5) ______
GENERAL COMPLETENESS
a) Conciseness and neatness (5) ______
TOTAL (100) ______
Table of Contents
Executive Summary ................................................................................................................................ 1
Introduction ............................................................................................................................................. 2
Objective ................................................................................................................................................. 3
Chemicals used ....................................................................................................................................... 3
Experimental Set-up................................................................................................................................ 3
Procedure ................................................................................................................................................ 4
Preparation of dye solution ................................................................................................................. 4
Concentration-adsorbance curve using UV spectrometer ................................................................... 4
Experimental Procedure ...................................................................................................................... 4
Observations and Calculations ................................................................................................................ 4
Results and Discussion ........................................................................................................................... 6
Conclusion .............................................................................................................................................. 7
References ............................................................................................................................................... 7
Acknowledgement .................................................................................................................................. 7
Appendix A8 ........................................................................................................................................... 8
Observation ......................................................................................................................................... 8
Detailed calculation ............................................................................................................................ 9
Sample Calculation ........................................................................................................................... 10

List of Figures
Figure 1: Experimental - Set-up .............................................................................................................. 3
Figure 2: Absorbance v/s concentration curve for Rhodamine B ........................................................... 5
Figure 3: Best fit of the data obtained ..................................................................................................... 5
Figure 4: RTD curve at different flowrates in a PFR .............................................................................. 6

List of Tables
Table 1: Absorbance data obtained at various concentrations ................................................................ 4
Table 2: Results Obtained ....................................................................................................................... 6
Table 3: Observation for flowrate 2600MLPH ....................................................................................... 8
Table 4: Observation for flowrate 3800MLPH ....................................................................................... 8
Table 5: Observation at flowrate 5400MLPH......................................................................................... 8
Table 6: Calculations for 2600MLPH..................................................................................................... 9
Table 7: Calculation for 3800MLPH ...................................................................................................... 9
Table 8: Detailed Calculation for flowrate 5400MLPH ....................................................................... 10
Executive Summary
The objective of this experiment was to study the residence time distribution in a PFR using
pulse input. The objective was achieved by using a PFR of volume 0.5Land Rhodamine B as
the tracer. To carry out the experiment water was made to flow through the PFR at three
different flowrates (2600, 3800, 5400 MLPH). Once the steady state was reached the tracer
was injected into the PFR. Then after regular intervals samples were collected from the outlet
of the PFR and the absorbance of the sample was measured using UV spectrometer. The
concentration of the tracer was calculated using the absorbance data obtained. On calculating
the concentrations it was found that as the flowrate increases the concentration at a particular
time decreases. The spread of the E curve was also found to decrease with increase in the
flowrate. For 2600, 3800 and 5400 MLPH mean residence time was calculated to be
3.271min, 2.903min and 2.346min respectively, the dispersion number was found to be
0.341, 0.370 and 0.346 respectively indicating slight deviation from plug flow.

1
Introduction
Different elements of fluid may take different routes through the reactor and so it might take
different length of time to pass through the vessel. The distribution of these times for the
stream of fluid leaving the vessel is called exit age distribution, E or the residence time
distribution.[1] It has units of time-1. The residence time distribution curve is for closed vessel
boundary condition i.e. the fluid only enters and leaves the vessel one time, so there should
be no flow or diffusion at the entry and exit. [1]
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.
a. Pulse Input
In a pulse, a one shot injection, N0 of the tracer is put in the feed stream entering the
reactor in a short duration of time. The outlet concentration is then measured as a function
of time. To measure the concentration, a UV spectrometer is used. The effluent
concentration-time curve is known as the C curve in the RTD analysis. If we assume a
sufficiently small time interval Δt at which concentration is C(t) which is exiting between
t and t + Δt, then this concentration is essentially constant. The amount of tracer leaving
the reactor would be given by:
∆𝑁 = 𝐶(𝑡)𝑣∆𝑡 … … … … … … … (6.1)
Where,
ΔN = tracer leaving the reactor
C(t) = concentration between t and t+Δt
v = effluent volumetric flowrate
∆𝑁 𝐶(𝑡)𝑣∆𝑡
= … … … … … … (6.2)
𝑁0 𝑁0
For a pulse we define,
𝑣𝐶(𝑡)
𝐸(𝑡) = … … … … … … … (6.3)
𝑁0
∆𝑁
𝐸(𝑡) = … … … … … … . (6.4)
𝑁0 ∆𝑡
𝑑𝑁 = 𝑣𝐶(𝑡)𝑑𝑡
∞
𝑁0 = ∫ 𝑣𝐶(𝑡)𝑑𝑡 … … … … … … (6.5)
0

2
 𝐶(𝑡)
𝐸(𝑡) = ∞ … … … … … … . (6.6)
∫0 𝐶(𝑡)𝑑𝑡
The variance is defined as:

𝜎 2 = (∑ 𝑡𝑖2 𝐶𝑖 ∆𝑡𝑖 )/( ∑ 𝐶𝑖 ∆𝑡𝑖 ) − 𝑡2 … … … … . . (6.7)

The dispersion number is given as:

𝜎2 𝐷 𝐷 2 𝑢𝐿
𝜎𝜃2 = = 2 ( ) − 2 ( ) (1 − exp 𝐷 ) … … … … … … … … (6.8)
𝑡 𝑢𝐿 𝑢𝐿
The RTD is used to characterize a real reactor and then use this to predict the exit conversion
and concentration reactions occur in the reactor. For this experiment we study the RTD in a
PFR of volume 0.5L using a pulse input and Rodamine-B as the tracer.

Objective
The objective of the experiment is to study the residence time distribution in a PFR using
pulse input.
Chemicals used
 Rhodamine B manufactured by Loba Chemie Pvt. Ltd.
Experimental Set-up
The experimental set-up is as shown in Fig. 1. The set-up is manufactured by Leiesil
Innovative System. There is a feed tank at the top to store water. The storage tank is
connected to a rotameters to measure the flow-rate of water entering the PFR. The PFR is
filled with beads and has a volume of 0.5L. The outlet is connected to a valve to drain the
water contained in the PFR.

Figure 1: Experimental - Set-up

3
Procedure
Preparation of dye solution
1. Measure and take 0.03g of Rhodamine B
2. Take 30mL of water.
3. Add 0.03g of Rhodamine B to 30mL of water to make 1000ppm solution.
4. Take 6ml of 1000ppm solution and add 24ml of water to it to make 200ppm solution.
Concentration-adsorbance curve using UV spectrometer
1. Solution of different concentration (0,1,2,3,4,5,6 and 7 ppm) of dye are made.
2. The absorbances of the solutions are measured using UV-Spectrometer.
3. Absorbance v/s concentration curve is plotted.

Experimental Procedure
a. Fill water in one of the feed tanks.
b. Set a flowrate of water using the rotameters provided.
c. Let water flow through the PFR
d. 10 minutes after steady state is achieved, add 10ml of the tracer Rodamine-B in the
PFR.
e. 1minute after the tracer is added take out 10 mL of mixture from the PFR and
measure the absorbance using UV spectrometer.
f. Continue taking the samples till water coming out of the PFR becomes clear i.e. free
of dye.
Observations and Calculations
 Absorbance data obtained at various concentration is shown in Table 1 and Fig. 2
shows the curve of absorbance v/s concentration for Rhodamine B.
Table 1: Absorbance data obtained at various concentrations

Conc Absorbance
0 0
1 0.093
2 0.184
3 0.291
4 0.393
5 0.53
6 0.652
7 0.775
8 0.871
9 1.026

4
 1.2

0.8
Absorbance

0.6

0.4

0.2

0
0 1 2 3 4 5 6 7 8 9 10
Concentration (ppm)

Figure 2: Absorbance v/s concentration curve for Rhodamine B

As it can be seen fromFig.2 that the data obtained almost fits in a straight line, it is verified
using Fig.3. Fig. 3 shows the best fit for the data obtained. As it can be seen that R 2 value is
almost equal to 1 it means that the data fits a linear curve quite well as R2 =1 means linear fit.
The equation of the straight line thus obtained is also shown in Fig. 3.
1.2

1 y = 0.1143x - 0.0327
R² = 0.9964

0.8
Absorbance

0.6

0.4

0.2

0
0 1 2 3 4 5 6 7 8 9 10
-0.2
Concentration (ppm)

Figure 3: Best fit of the data obtained

5
Results and Discussion
The objective of the experiment was to carry out RTD studies in a PFRusing a pulse input.
The study was carried out using Rhodamine-B as the tracer and a PFR of volume 0.5L as was
shown in Fig. 1. Fig. 4 shows the RTD curve obtained for each of the flow-rate (2600,3800,
5400 MLPH). The data and the detailed calculations are available in Appendix A8.

0.6

0.5

0.4

At 2600MLPH
0.3
E

At 3800MLPH

0.2 At 5400 MLPH

0.1

0
0 2 4 6 8 10 12
time(min)

Figure 4: RTD curve at different flowrates in a PFR

As can be seen from Fig. 4 as the flowrate increases the concentration at a particular time
decreases. The spread of the E curve also decreases with increase in the flowrate. Higher the
flowrate faster the dye leaves the PFR. . It can be seen that a dome shaped curve is obtained.
The tracer concentration changes with respect to time but no reaction takes place. RTD
depends on the mixing pattern of the reactor. Since, there is radial and axial diffusion taking
place in the packed bed reactor which leads to the area to increase. Under true plug flow
condition (i.e. no axial mixing), the tracer will come out as soon as it enters the reactor.

It was also required to find out the mean residence time, the variance and the dispersion
number. Table 2 shows the value of these parameters that were obtained.
Table 2: Results Obtained

2600MLPH 3800MLPH 5400MLPH

Mean Residence Time 3.271 2.903 2.346
(min)
Variance 7.301 6.233 4.009

6
 Dispersion number 0.341 0.370 0.346
Volume (L) 0.142 0.184 0.211

The variance is used to define the spread of the curve. The dispersion number is used to
determine the extent of axial dispersion. If this number reaches infinity it shows a large
dispersion and mixed flow condition. If this number reaches to almost zero it shows a small
dispersion and hence plug flow [1]. The actual volume of the PFR is 0.5L while that calculated
is quite less than 0.5L. In this case since the PFR used in the experiment is filled with beads it
might be behaving as a fixed bed reactor instead of a PFR and hence the deviation in the
value of volume obtained. The average error in volume of PFR calculated is 64.2%
Conclusion
The aim of the experiment was to study the RTD in a packed bed reactor and find out
important parameters related to RTD. The dispersion number is slightly more than 0 showing
a slight deviation from plug flow. The actual volume of the PFR used is 0.5L while the
volume calculated is quite less than 0.5L that can be seen in table 2. So, it can be concluded
that case since the PFR used in the experiment is filled with beads it might be behaving as a
fixed bed reactor instead of a PFR and hence the deviation in the value of volume obtained
and the dispersion number.
References
1. O. Levinspiele, “Chemical Reaction Engineering” 2nd edition, John Wiley and Sons,
2007, 319-421
Acknowledgement
I would like to thank all my group members Bodawar Narendra and Yash Gupta, for their co-
operation and contributions while performing the experiment. I would also like to thank
Ananta Bhatnagar and Sriraj Mestry for helping us in making the dye solution. . I would also
like to thank few other classmates Heena Goyal, Gopika Menon, Harshit Shah and Mustafa
Barwaniwala for sharing their absorbance-concentration data of Rodamine B with us.

7
Appendix A8
Observation
Table 3: Observation for flowrate 2600MLPH

Flow rate time 1st set 2nd set Avg. absorbance

2600 0 0 0 0
2600 1 1.275 1.135 1.205
2600 2 0.792 0.71 0.751
2600 3 0.395 0.383 0.389
2600 4 0.3 0.243 0.2715
2600 5 0.193 0.142 0.1675
2600 6 0.145 0.115 0.13
2600 7 0.11 0.105 0.1075
2600 8 0.087 0.087 0.087
2600 9 0.079 0.066 0.0725
2600 10 0.06 0.05 0.055
2600 11 0.056 0.046 0.051

Table 4: Observation for flowrate 3800MLPH

Flow rate time 1st set 2nd set Avg. absorbance

3800 0 0 0 0
3800 1 1.073 1.06 1.0665
3800 2 0.394 0.404 0.399
3800 3 0.211 0.238 0.2245
3800 4 0.153 0.142 0.1475
3800 5 0.101 0.102 0.1015
3800 6 0.07 0.074 0.072
3800 7 0.055 0.052 0.0535
3800 8 0.044 0.046 0.045
3800 9 0.036 0.042 0.039
3800 10 0.034 0.037 0.0355

Table 5: Observation at flowrate 5400MLPH

Flow rate time 1st set 2nd set Avg absorbance

5400 0 0 0 0
5400 1 0.817 0.815 0.816
5400 2 0.189 0.188 0.1885
5400 3 0.096 0.097 0.0965
5400 4 0.06 0.058 0.059
5400 5 0.039 0.039 0.039

8
5400 6 0.03 0.03 0.03
5400 7 0.025 0.025 0.025
5400 8 0.021 0.022 0.0215

Detailed calculation
Table 6: Calculations for 2600MLPH

time t2 Avg absorbance Concen-tration Area under C curve E

0 0 0 0.281 31.921 0.009
1 1 1.205 10.851 31.921 0.340
2 4 0.751 6.868 31.921 0.215
3 9 0.389 3.693 31.921 0.116
4 16 0.2715 2.662 31.921 0.083
5 25 0.1675 1.750 31.921 0.055
6 36 0.13 1.421 31.921 0.045
7 49 0.1075 1.224 31.921 0.038
8 64 0.087 1.044 31.921 0.033
9 81 0.0725 0.917 31.921 0.029
10 100 0.055 0.763 31.921 0.024
11 121 0.051 0.728 31.921 0.023

Table 7: Calculation for 3800MLPH

time t2 Avg absorbance Concen-tration Area under C curve E

0 0 0 0.281 21.965 0.009
1 1 1.0665 9.636 21.965 0.439
2 4 0.399 3.781 21.965 0.172
3 9 0.2245 2.250 21.965 0.102
4 16 0.1475 1.575 21.965 0.072
5 25 0.1015 1.171 21.965 0.053
6 36 0.072 0.912 21.965 0.042
7 49 0.0535 0.750 21.965 0.034
8 64 0.045 0.675 21.965 0.031
9 81 0.039 0.623 21.965 0.028
10 100 0.0355 0.592 21.965 0.027

9
Table 8: Detailed Calculation for flowrate 5400MLPH

time t2 Avg absorbance Concen-tration Area under C curve E

0 0 0 0.281 10.635 0.009
1 1 0.816 5.889 10.635 0.554
2 4 0.1885 1.531 10.635 0.144
3 9 0.0965 0.892 10.635 0.084
4 16 0.059 0.632 10.635 0.059
5 25 0.039 0.493 10.635 0.046
6 36 0.03 0.431 10.635 0.040
7 49 0.025 0.396 10.635 0.037
8 64 0.0215 0.372 10.635 0.035

Sample Calculation
For flowrate of 2600MLPH

At t=1 min

1.275 + 1.135
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑎𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 = = 1.205
2

Using straight line equation for absorbance concentration data:

1.205 + 0.031
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 = = 10.851
0.114

Similarly concentration at the rest of the time was calculated

𝐴𝑟𝑒𝑎 𝑢𝑛𝑑𝑒𝑟 𝑡ℎ𝑒 𝐶 𝑐𝑢𝑟𝑣𝑒 = ∑ 𝐶𝑖 ∆𝑡𝑖 = (10.85 + 6.86 + 3.69 + 2.66 + 1.75 + 1.42 + 1.224 +
1.044 + 0.917 + 0.763 + 0.728) × 1 = 31.921

𝐶 10.851
𝐸= = = 0.009
𝐴𝑟𝑒𝑎 𝑢𝑛𝑑𝑒𝑟 𝐶 𝑐𝑢𝑟𝑣𝑒 31.921

Similarly the value of E at various time was calculated

∑ 𝐶𝑖 𝑡𝑖 ∆𝑡𝑖
𝑡= ∑ 𝐶𝑖 ∆𝑡𝑖
=
(10.85×1+6.86×2+3.69×3+2.66×4+1.75×5+1.42×6+1.224×7+1.044×8+0.917×9+0.763×10+0.728×11)
(10.85+6.86+3.69+2.66+1.75+1.42+1.224+1.044+0.917+0.763+0.728)
= 3.271

∑ 𝐶𝑖 𝑡𝑖2 ∆𝑡𝑖
𝜎2 = ∑ 𝐶𝑖 ∆𝑡𝑖
− 𝑡2 =
(10.85×1+6.86×4+3.69×9+2.66×16+1.75×25+1.42×36+1.224×49+1.044×64+0.917×81+0.763×100+0.728×121)
(10.85+6.86+3.69+2.66+1.75+1.42+1.224+1.044+0.917+0.763+0.728)
−
3.2712 = 7.301
𝜎2
𝐷𝑖𝑠𝑝𝑒𝑟𝑠𝑖𝑜𝑛 𝑛𝑢𝑚𝑏𝑒𝑟 = = 0.341
2𝑡 2
2600 × 3.271
𝑉𝑜𝑙𝑢𝑚𝑒 = = 0.142𝐿
60000

10