CDB 3052 Chemical Engineering Laboratory II Jan 2016

Experiment 3 RTD in Packed Bed

Lab Instructor : Haswin Kaur

Group Members

:
N

Name

ID

o
1

Maryam binti Nasaruddin

19076

Sugentther A/L Chantravarnam

19054

Nur Kamarul Syaabah Ng binti Mohamad

19155

Hafiz

1.0 OBJECTIVES

Abdul Aiman bin Abdul Latif

19310

Wan Intan Nadiah binti Borharuddin

18857

In this experiment, we are using tubular reactor to evaluate the residencetime distribution (RTD) in packed bed. Packed Bed reactor consists of
mainly a vertical glass column packed with glass Raschig rings. The effect
of liquid (L) and gas (G) feed rates on the mean residence time and
degree (intensity) of liquid-phase axial dispersion is evaluated during this
experiment.
We will observe two modes of the experiment which are mode and pulse.
Each mode consists of two different flow which are co-current flow where
both gas and liquid flows in the same direction and counter-current flow
where both liquids flow on the opposite direction to each other. The
conductivity of NaCl solution is recorded and RTD is evaluated by the
calculation based on the conductivity and concentration of NaCl.

2.0 THEORY
The residence time distribution (RTD) of a chemical reactor is a probability
distribution function that describes the amount of time a fluid element
could spend inside the reactor. Chemical Engineers use the RTD to
characterize the mixing and flow within reactors and to compare the
behavior of real reactors to their ideal models. This is useful, not only for
troubleshooting existing reactors, but in estimating the yield of a given
reaction and designing future reactors.
The RTD is determined experimentally by injection an inert chemical,
molecule, or atom, called a tracer, into the reactor at some time t = 0 and
then measuring the tracer concentration, C, in the effluent stream as a
function of time. In addition to being a nonreactive species that is easily
detectable, the tracer should have physical properties similar to those of
the reacting mixture and be completely soluble in the mixture. It is also
should not adsorb on the walls or other surfaces in the reactor. The latter
requirements are needed so that the tracers behavior will honestly reflect
that of the material flowing through reactor.
The two most used methods of injection are pulse input and step input.

3.0 EXPERIMENT DESIGN

3.1 Experiment A: The effect of step change input
a) Counter-current Mode
1. Firstly, we perform the general start-up procedure.
2. Valves V3, V5 and V10 remain closed for counter-current
mode.
3. Valve V1 was opened and pump P1 was switch on. The column
was filled up with de-ionized water to packing height.
4. Valve V1 was adjusted to obtain a liquid flowrate of 500
ml/min.
5. Valve V6 and V8 was opened to obtain a gas flow rate of 1.0 L
min-1.
6. Observe the conductivity reading of CT1 and let it stabilizes at
low value.
7. Dosing pump P2 was switch on and valve V14 was open to
bleed off any air trapped in the tubing.
8. Close valve V14. Open valve V9 and start timer
simultaneously. Conductivity reading CT1 at 1 min interval is
recorded.
9. Continue recording until conductivity reading is constant.
10.
Stop the experiment and drain out all liquid from the
system.

b) Co-current Mode
1. Firstly, we perform the general start-up procedure.
2. Valves V2, V4 and V9 remain closed for co-current mode while
valves V3 and V5 is opened.
3. Pump P1 is switched on.Open and adjust valve V1 to obtain a
liquid flowrate of 500 ml/min.
4. Open valve V6. Open valve V8 to obtain a gas flowrate of 1 Lmin
5. Observe the conductivity reading of CT2 and let it stabilizes at
low value.
6. Dosing pump P2 was switched on and valve V15 was open to
bleed off any air trapped in the tubing.
7. Close valve V15. Open valve V10 and start timer simultaneously.

Record conductivity reading CT2 at 1 min interval.

8. Continue recording until conductivity reading is constant.
9. Repeat the experiment with gas flow rate of 2.0 L min-1. Ensure
that the system is flushed with de-ionized water until no traces of
salt is detected.
10. Stop the experiment and drain out all liquid from the system.

3.2 Experiment B: The effect of pulse input.

a) Counter-current Mode
1. Firstly, we perform the general start-up procedure.
2. Valves V3, V5 and V10 remain closed for counter-current mode.
3. Valve V1 was opened and pump P1 was switch on. The column was
filled up with de-ionized water to packing height.
4. Valve V1 was adjusted to obtain a liquid flowrate of 500 ml/min.
5. Valve V6 and V8 was opened to obtain a gas flow rate of 1.0 L min1.
6. Observe the conductivity reading of CT1 and let it stabilizes at low
value.
7. Dosing pump P2 was switch on for 2 minutes and valve V9 was close
and pump P2 was stopped.
8. Close valve V14. Open valve V9 and start timer simultaneously.
Conductivity reading CT1 at 1 min interval is recorded.
9. Continue recording until conductivity reading is constant.
10.

Stop the experiment and drain out all liquid from the system.

b) Co-current Mode
1. Firstly, we perform the general start-up procedure.
2. Valves V2, V4 and V9 remain closed for co-current mode while
valves V3 and V5 is opened.
3. Pump P1 is switched on.Open and adjust valve V1 to obtain a

4.
5.
6.
7.
8.
9.

liquid flowrate of 500 ml/min.

Open valve V6. Open valve V8 to obtain a gas flowrate of 1 Lmin
Observe the conductivity reading of CT2 and let it stabilizes at
low value.
Dosing pump P2 was switched on for 2 minutes and valve V10
was close and pump P2 was stopped.
Close valve V15. Open valve V10 and start timer simultaneously.
Record conductivity reading CT2 at 1 min interval.
Continue recording until conductivity reading is constant.
Repeat the experiment with gas flow rate of 2.0 L min-1. Ensure

that the system is flushed with de-ionized water until no traces of

salt is detected.
10. Stop the experiment and drain out all liquid from the system.

4.0 Result
Experiment A: The Effect of step change input

Graph of Concentration (g/L) vs Time (min)

10

12

14

16

Time (min)
Counter-Current

Co-Current

Figure 1 : Graph of Concentration vs Time

E(t) vs Time (min)

12
10
8
E(t)

6
4
2
0
0

Time (min)
Counter-Current

Co-Current

Figure 2 : Graph of E(t) vs Time

10

12

Mean residence time, tm

Spread of the
distribution, 2
Skewness, s3

Counter Current

Co Current

0.720358274

1.535219971

3.73209223

10.0449582

8.927674664

15.62597979

Table 1: Result of Experiment A

Experiment B: The effect of pulse input

Concentration (g/L) vs Time (min)

12
10
8
Concentration (g/L)

6
4
2
0
0

Time (min)
Counter-Current

Co-Current

Figure 3 : Graph of Concentration vs Time

E(t) vs Time (min)

12
10
8
E(t)

6
4
2
0
Counter-Current

Co-Current

Figure 4 : Graph of E(t) vs Time

10

12

Mean residence time,

tm
Spread the distribution,
2
Skewness, s3

Counter- current

Co- current

7.554317

5.26888

1.653922

0.189226

-6.35778

-50.5967

Table 2 : Result of Experiment B

5.0 CALCULATION

1. Converting conductivity into concentration

Using the equation of graph of Concentration (g/L) vs Conductivity
(micro s) :
y=1634.5 x+ 483.51
Example
At time = 1 min for step

, Conductivity = 377

377483.51
1634.5

Concentration =

= - 0.06516

2. Calculating fraction residence time by using the formula below;

For Pulse-input :
E (t)=

C (t)

C (t) dt
0

Where,

C (t)dt=area under the graph

0

18

C (t) dt=
0

6.381878

Example:
At time =1 min
E (t)=

C (t )

C ( t ) dt
0

0.06223
6.381878

0.00975

For Step- input :

E (t)=

[ ]

d C (t)
dt Co

C o= of all concentration
Example :
t = 2 min
E (t)=

d 0.0664
dt 18.55

= - 0.0000659

3. Calculating mean residence time by using this formula,

t m= tE (t)dt
0

Example:
18

t m= tE (t)dt
0

0.720358274

4. Calculating the variance,

= ( tt m )2 E ( t ) dt
2

Example:
18

2= ( tt m )2 E ( t ) dt
0

= 3.73209223

5. Calculating skewness,

1
s = 3 /2 ( tt m )3 E(t )dt
0
3

Example:
18

1
s = 3 /2 ( tt m )3 E(t )dt
0
3

s 3= 8.927674664

6. Proving that,

E ( t ) dt=fraction of effluent which has beenreactor less thantimet=F (t)

0

F ( t )=1

6.0 DISCUSSION

In this experiment we did two sub-experiments which are Experiment

A( Effect of Step change Input ) and Experiment B ( Effect of Pulse Input ).
From the conductivity values that we recorded during the experiment, the
data was elaborated to find concentration of tracer ,C(t) and residence
time distribution,E(t).Then we plotted the graphs for C(t) and E(t) against
Time. From the conductivity also we further develop and able to calculate
concentration, mean residence time, variance and skewness.

Based on the graphs in experiment A, residence time distribution in

counter-current mode is larger than co-current mode. In counter-current
mode, the tracer takes a shorter time to detect the tracer. From the
experiment A which we set 1.0L/min liquid flow rates, the variance, mean
residence time and skewness in counter-current mode is lower compared
to the co-current mode.The graph of E(t) vs time, concentration of the
tracer should increase with time as the tracer is injected continuously with
constant amount of tracer throughout the experiment. But due to some
miscalculation and error,we did not manage to get that type of

graph.Based on the graphs shown in result of experiment B, the pattern of

all graphs are almost the same; bell-shape trend. It depicts the sudden
injection of tracer into the feed stream entering the reactor.

From both experiment B for counter current flow and co-current flow, the
mean residence time is longer in counter current flow.According to the
theory, the mean residence time should be shorter if the flow rate is high
which is contradict with our result. This might caused by some error
during the experiment. To compare between two different type of flow
which are counter current and co-current mode, the mean residence time
for co-current flow is longer than that of counter current flow.

This is because in counter current flow the sensor will take a shorter time
to detect the tracer during the counter flow from gas and liquid. Skewness
is a measure of the asymmetry of the probability distribution of a real
system to its mean. In addition, skewness is also higher for co-current flow
and lower for counter current flow.

7.0 CONCLUSION
Based on the experiment, we had successfully achieved all the objectives.
The effect of step input (experiment A) and pulse input (experiment B) can
be observed from the graphs of concentration C(t) vs time plotted.
In experiment A (step input), method of continuously injection, tracer
shows higher concentration and lower residence time distribution in
counter current mode compared to co current mode.In counter-current,
the tracer takes shorter time to fully circulate throughout the reactor
which causes perfect mixing faster compared to co-current flow which
takes longer to circulate throughout the reactor. When opposed, the fluid
is forced to move outwards and circulate faster.In co-current, the fluid
flows in the same direction, thus it takes time for the tracer to be fully
circulated in the reactor.

For counter current mode, the mean residence time and variance are
lower than co current mode. This indicates that the tracer in counter

current mode spends less time in the reactor and lesser distributions
spread.The skewness in counter current is lower than co current. This
shows that the distribution is skewed in one direction or another in
reference to the mean more than the co current.

Based on the graphs shown in result of experiment B, the pattern of all

graphs are almost the same; bell-shape trend. It depicts the sudden
injection of tracer into the feed stream entering the reactor. The result of
distribution is recorded to measure which method distributes the tracer in
a much shorter time in the reactor. In this experiment, counter-current
distributes the tracer much in a shorter time compared to co-current. This
is because in counter-current flow, the fluid flows against air, thus causing
more thorough mixing.

8.0 REFERENCE
K. Saroha, K. D. P. Nigam, K. Saxe and D. Lalji. (1998). The Canadian
Journal of Chemical Engineering: RTD Studies in Trickle Bed Reactors
Packed with Porous Particles. Vol. 76.
Asnizam, H ., Chemical Engineering Laboratory II : RTD in Packed Bed
(2013), 1-15.

Time(min
)

Conductivit
y

Concentration
(g/L)

F(t)

E(t)

tE(t)

377

-0.0651637

-0.00351

375

-0.0663873

-0.00358

-6.59768E-05

405.4

-0.0477883

0.001002848

797.1

0.19185684

1851.4

0.8368859

2858.7

1.45315999

3293.2

1.71899052

3647.2

1.93557051

3802.6

2.03064546

-0.00258
0.01034
5
0.04512
5
0.07835
4
0.09268
7
0.10436
5
0.10949
2

-0.00013
0.00300
9
0.05168
6
0.17389
8
0.19937
5
0.10033
4
0.09342
3
0.04613
8

0.012921565
0.034779693
0.033229237
0.014333469
0.011677901
0.005126401

tm
-6.59768E05
0.00143829
5
0.02734740
2
0.11279236
3
0.18663694
6
0.14985485
5
0.09687874
8
0.06978040
9
0.03748474
4

(ttm)E
0

-0.000
0.005
2
0.138
5
0.637
2
0.926
2
0.565
5
0.618
9
0.351
7

0.11237
5

10

3890

2.08411747

11

3932.6

2.11018048

12

3946.8

2.11886816

13

3949.9

2.12076476

14

3955.9

2.12443561

0.11378
0.11424
8
0.11435
1
0.11454
9

18.5461364

0.002883188
0.001405307
0.000468436
0.000102264
0.000197931
0.11806226
3

0.02883
2
0.01545
8
0.00562
1
0.00132
9
0.00277
1

0.02214512
8
0.01053980
1
0.00347533
0.00205023

0.248
6

0.14
0.059
9

0.015
0.034
5

0.7203582
74

Experiment A Counter Current

Experiment A Co Current
Time(mi Conductiv
n)
ity
1

179.9

Concentrati
on
(g/L)
-0.185751

176.2

-0.1880147

190.3

-0.1793882

240

-0.1489813

452.9

-0.0187274

753.1

0.16493729

1147.4

0.40617314

1470.9

0.60409299

1778.4

0.79222392

10

2119.9

1.00115632

11

2358.4

1.1470725

12

2502.5

1.23523402

13

2521.3

1.246736

F(t)
0.0216
8
0.0219
4
0.0209
4
0.0173
9
0.0021
9
0.0192
49
0.0474
02
0.0705
0.0924
55
0.1168
39
0.1338
68
0.1441
56
0.1454
99

(ttm)E(
)

E(t)

tE(t)

0
0.000264
181

tm
0.000264
181

0.00053

0.001245
935

-5.7E05

0.001006
744

0.00302

0.008607
302

0.0021
6

0.003548
593

0.01419
4

0.045099
978

0.0215
58

0.015201
117
0.021434
36
0.028153
125
0.023097
986
0.021955
582
0.024383
191
0.017028
964
0.010288
778
0.001342
325

0.07600
6
0.12860
6
0.19707
2
0.18478
4

0.102305
872
0.162839
018
0.190927
883
0.191192
064
0.220716
074
0.215575
255
0.155391
97
0.070457
783
0.087943
708

0.1824
85
0.4272
78
0.8407
6
0.9653
43
1.2234
3
1.7471
17
1.5254
9
1.1267
41
0.1764
37

0.1976
0.24383
2
0.18731
9
0.12346
5
0.01745

14

2679.8

1.34370756

15

2687.2

1.34823493
8.5687060
3

0.1568
16
0.1573
44

0.011316 0.15843 0.083181

942
7
311
0.000528 0.00792
362
5
0.179021
1.535219
1
888
971

1.7583
22
0.0957
92

Experiment B Counter Current

Time(mi
n)

Conductiv
ity

Concentration(
g/L)

381.8

-0.06222698

383.1

-0.06143163

tE(t)
0.0097
5
0.0192
5
0.0124
8

-0.0145
0.0158
7
0.0520
81

(t
tm)
)
0.41
8
0.29
6
0.08
2

440.1

-0.02655858

Integral
E(t)
0.0618 0.00975057
3
5
0.00962594
-0.044
9
0.0797 0.00416156
74
2

787.7

0.186105843

0.4691
28

0.02916161
1

0.1166
46

0.3529
66

0.36
04

1712.9

0.752150505

0.9606
55

0.11785723
6

0.5892
86

0.8442
42

0.76
64

1.2214
68

0.18319979
9

1.0991
99

1.2481
75

0.44
93

1.2018
6
1.0137
29
0.7788
87
0.4921
32
0.2473
78
0.1209
79
0.0423
92
0.0064
3

0.19959295
9
0.17705476
0.14063510
1
0.10345809
8
0.05076990
5
0.02675536
3
0.01115789
4

1.3971
51
1.4164
38
1.2657
16
1.0345
81
0.5584
69
0.3210
64
0.1450
53

0.06
28
0.03
69
0.29
27
0.61
21
0.60
77
0.52
96
0.33
93

0.00212727
6

0.0297
82

1.4067
94
1.3410
77
1.1501
48
0.7965
25
0.4397
67
0.2330
58
0.0874
17
0.0161
8

2394.5

1.169158764

2565.5

1.273777914

2330.4

1.129941878

1950.5

0.89751606

10

1562.7

0.660256959

11

1013.1

0.324007342

12

762.6

0.170749465

13

599.9

0.071208321

14

505.7

0.013576017

tm

0.08
82

15

440.3

-0.02643622

16

415.2

-0.0417926

17

400.6

-0.05072499

18

390.3

-0.05702661

0.0341
1
0.0462
6
0.0538
8

0.00414238
9
0.00654863
6
0.00794828
6
0.00893571

0.0621
4
0.1047
8
0.1351
2
0.1608
4

6.3818 0.9906568
78
96

0.0834
6
0.1199
5
0.1479
8

0.22
5
0.46
1
0.70
5

-0.9
7.5543
17

Experiment B Co- Current

-0.09532579

Integra
l
0.0320
6

E(t)
0.05702462
7

tE(t)
0.0570
2

tm
0.0098
5

(ttm)
)
1.03
8

534.5

0.031196084

0.1304
62

0.01866174

0.0373
23

0.2247
99

0.19
11

859

0.229727745

0.2783
05

0.13742492
2

0.4122
75

0.5972
25

0.70
38

0.3450
84

0.19554385
4

0.7821
75

0.9343
88

0.31
37

0.3318
08
0.2871
77
0.2287
79
0.1303
09
0.0564
03
0.0099
66
0.0283
6

0.21732015
4
0.17965996
5

1.0866
01
1.0779
6
1.1474
57
0.8783
42
0.4149
98
0.2137
01
0.1039
1

1.0822
8
1.1127
09

0.01
11
0.09
35
0.49
39
0.81
46
0.64
21
0.47
37
0.31
7

Time(mi
n)

Conductiv
ity

Concentration(
g/L)

327.7

2
3
4

1017.8

0.326882839

1077.3

0.363285408

974.4

0.300330376

931.4

0.274022637

783.5

0.18353625

609.5

0.077081676

10

541.9

0.035723463

11

457.7

-0.01579076

0.16392247
0.10979281
1
0.04611085
8
0.02137005
3
0.00944615
6

1.0129
0.6466
7
0.3143
49
0.0548
96
0.1988
8

12

416.6

-0.04093607

13

334

-0.0914714

0.02448827
-0.0662
3
0.05471890
1
1.6716
61

0.2938
6
0.7113
5

0.5026

5.268
88

1.10
1
3.27
6