ARTICLE IN PRESS

Applied Radiation and Isotopes 67 (2009) 12481253

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Applied Radiation and Isotopes

journal homepage: www.elsevier.com/locate/apradiso

Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed
sieve plate extraction column using radiotracer technique
Ghiyas Ud Din a,c,, Imran Raq Chughtai b, Mansoor Hameed Inayat b, Iqbal Hussain Khan c
a
Department of Nuclear Engineering, Pakistan Institute of Engineering and Applied Sciences [PIEAS], P.O Nilore, Islamabad, Pakistan
b
Department of Chemical and Materials Engineering, Pakistan Institute of Engineering and Applied Sciences [PIEAS], P.O Nilore, Islamabad, Pakistan
c
Isotope Application Division, Pakistan Institute of Nuclear Science and Technology [PINSTECH], P.O Nilore, Islamabad, Pakistan

a r t i c l e in f o a b s t r a c t

Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental
Keywords: importance in the design and operation of liquidliquid extraction pulsed sieve plate columns have
Liquidliquid extraction been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for
Pulsed sieve plate column a range of pulsation frequency and amplitude in a liquidliquid extraction pulsed sieve plate column
Residence time distribution (RTD) with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was
Axial mixing operated in emulsion region and 99mTc in the form of sodium pertechnetate eluted from a 99Mo/99mTc
Holdup generator was used to trace the dispersed phase. Axial dispersed plug ow model with openopen
Slip velocity
boundary condition and two points measurement method was used to simulate the hydrodynamics of
Radiotracer
dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases
with increase in pulsation frequency and amplitude until a maximum value is achieved while slip
velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum
value. Short lived and low energy radiotracer 99mTc in the form of sodium pertechnetate was found to be
a good water tracer to study the hydrodynamics of a liquidliquid extraction pulsed sieve plate column
operating with two immiscible liquids, water and kerosene. Axial dispersed plug ow model with
openopen boundary condition was found to be a suitable model to describe the hydrodynamics of
dispersed phase in the pulsed sieve plate extraction column.
& 2009 Elsevier Ltd. All rights reserved.

1. Introduction as much as 30% (Li and Ziegler, 1967). The major sources of axial
mixing in the extraction columns are geometrical and operating
Liquidliquid extraction is a process of separation of constitu- parameters. Therefore, the presence of axial mixing in such kind
ents of a liquid phase by contacting it with another immiscible of equipments is unavoidable and needs special care. A simple
liquid phase. Petroleum, nuclear, chemical, metallurgical, phar- approach to represent the hydrodynamics of phases in these kind
maceutical, food processing and bio-processing industries are the of columns is the axial dispersion model (ADM) (Levenspiel and
major beneciaries of this technology. Column type contactors Smith, 1957; Levenspiel, 1999) and the concept of residence time
with agitation are very famous liquidliquid extraction equip- distribution (RTD) analysis is an important method for the
ments as they offer large interfacial area, high mass transfer estimation of axial dispersion in chemical reactors (Danckwerts,
coefcient, high turbulence and minimum radial gradients. 1953). The holdup and slip velocity of dispersed phase are other
Counter current movement of phases in these type of columns parameters of fundamental importance that need to be focused in
provide high concentration gradients for efcient mass transfer the design and operation of pulsed extraction columns.
but axial mixing in both phases lowers the process efciency by Axial mixing in the continuous phase of liquidliquid extrac-
lowering solute concentration gradients. It has been reported that tion columns remained a major focus of many studies. These
axial mixing in extraction columns lowers the process efciency include studies on spray towers (Hazlebeck and Geankoplis, 1963;
Henton and Cavers, 1970; Geankoplis et al., 1982), reciprocating
plate extraction columns (Kim and Baird, 1976a, b; Hafez et al.,
1979; Parthasarathy et al., 1984) and pulsed sieve plate extraction
 Corresponding author at: Department of Nuclear Engineering, Pakistan
columns (Kumar and Hartland, 1989). Axial mixing in the
Institute of Engineering and Applied Sciences [PIEAS], P.O Nilore, Islamabad,
Pakistan. Tel.: +92 51 2207381x3332; fax: +92 51 2208070.
dispersed phase of liquidliquid extraction columns has either
E-mail addresses: fac192@pieas.edu.pk, ghiyasuddin@hotmail.com been assumed negligible or it has not been estimated. Only a few
( Ghiyas Ud Din). studies can be found regarding axial dispersion in the dispersed

0969-8043/$ - see front matter & 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.apradiso.2009.02.024
 ARTICLE IN PRESS
Ghiyas Ud Din et al. / Applied Radiation and Isotopes 67 (2009) 12481253 1249

phase (Srinikethan et al., 1987) with conventional methods in proaches present some disadvantages including low sensitivity,
which a non-radioactive tracer is injected into the system and requirement of phase separation before measurement and poor
measurements were made by a conductivity probe. The holdup statistics. Most important of all is that one needs to shutdown the
and slip velocity of the dispersed phase have also been plant to obtain the holdup fraction at each operating parameter
determined by arresting the ow of phases and measuring the resulting in a high plant shutdown.
fractional dispersed phase volume in the extraction column Radiotracers are being used for industrial process optimization
(Venkatanarasaiah and Varma, 1998). These experimental ap- and trouble shooting from decades. They offer state of the art

Light phase outlet

Heavy phase inlet

Injection port
To collection vessel

D1
D2

Balance leg
From heavy phase feed vessel
via metering pump

To collection vessel

Ratemeters

Data
Acquisition
System

D3

Light
phase Interface
inlet level
Heavy phase
outlet

From light phase feed vessel

via metering pump Pulse unit

Fig. 1. Schematic diagram of pulsed sieve plate extraction column.

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1250 Ghiyas Ud Din et al. / Applied Radiation and Isotopes 67 (2009) 12481253

technology with high sensitivity, on-line measurement without Table 1

disturbing the plant operation, better statistics, high benet to Pulsed sieve plate extraction column specication and range of operating
variables.
cost ratio and possibility of getting information from remote
locations of process equipment. A variety of industrial process Internal diameter of the column (m) 5  102
investigations have been carried out using the power of radio- Length of the column (m) 2
tracer technology (Thyn et al., 2000; Thyn and Zitny, 2002; Pant Number of sieve plates 38
and Yelgoankar, 2002; Farooq et al., 2003; Kim et al., 2005). Plate spacing (m) 5  102
Plate diameter (m) 5  102
Although numerous applications can be found in literature Hole size (m) 2  103
regarding industrial process investigations using radiotracer Average number of holes 140 per plate
technology but only a few have been reported with reference to Average free area (%) 25
the hydrodynamics of liquidliquid extraction columns Dispersed phase supercial velocity (m/s) 0.34  102 and 0.44  102
Continuous phase supercial velocity (m/s) 0.37  102 and 0.47  102
(Arthayukti et al., 1976).
Range of pulsation frequency (s1) 0.72.0
The present investigations are focused to study the hydro- Range of pulsation amplitude (m) 0.8  1021.6  102
dynamics of dispersed phase in a pulsed sieve plate extraction
column using radiotracer RTD analysis. Effect of pulsation
frequency and amplitude have been studied on the axial mixing,
holdup and slip velocity of dispersed phase for two sets of
dispersed and continuous phase supercial velocities and the The tracer data from detectors D2 (column inlet) and D3
system was simulated using the ADM. (column outlet) was corrected for background, radioactive decay
and normalized. The experimental mean residence time (MRT) of
the system was calculated by the difference of rst moments of
outlet and inlet response curves. Mathematical expression for the
2. Materials and methods rst moment in discrete form can be written as
P
t C Dt
The schematic diagram of pulsed sieve plate extraction column First moment Pi i i i (1)
under investigation is shown in Fig. 1. The internal diameter of the i C i Dt i

column is 5  102 m and height is 2 m. Two separating chambers where C is the tracer concentration (counts/s in present case), t is
one at the top and the other at the bottom of the column are also the time of measurement (s), Dt is the time interval between the
part of this apparatus. The column is tted with regularly spaced two measurements (s), and i 0,1,2,3,y.
(5  102 m) sieve plates which help to increase the interfacial Overall holdup of the phase under investigation was calculated
area between the two immiscible liquids. The column was on the basis of calculated MRT using the following relationship:
operated counter currently with heavy phase (water) as
dispersed and light phase (kerosene) as continuous phase. The tQ d
Hd (2)
kerosene is fed into the lower separating chamber with the help of VR
a metering pump which then ows upwards through the sieve where Hd is the dispersed phase holdup, Qd is the dispersed phase
plate column to the upper separating chamber where it overows ow rate, t is the MRT, and VR is the effective reactor volume.
to a collection vessel. Similarly water is fed into the top separating The slip velocity of the dispersed phase averaged over the
chamber via a metering pump from where it ows downwards whole column was estimated from the above calculated Hd using
through the column to the lower separating chamber and then it the following equation (Venkatanarasaiah and Varma, 1998):
ows through a balance leg into a collection vessel. A pulse unit
Ud Uc
located at the base of lower separating chamber provides vertical Vs (3)
pulses to the owing uids. The column was operated in the Hd 1  Hd
emulsion regime i.e. dispersed phase remained dispersed where Vs is the slip velocity of dispersed phase, Ud is the dispersed
throughout the plate stack and no coalescence into layers phase supercial velocity, Uc is the continuous phase supercial
occurred at the plates. A liquidliquid interface was allowed to velocity.
form at about 10 cm below the light phase inlet and this interface The RTD is a probability distribution function that describes
level was stabilized with the help of a balance leg before starting the amount of time a uid element spends inside a reactor. It
an experiment. helps in troubleshooting of reactors and characterizes the mixing
99m
Tc in the form of sodium pertechnetate having half life of and ow within the reactors. If an impulse of tracer is injected at
6.02 h and gamma energy 0.14 MeV (91%) is a well known water the inlet of a system at time t 0 and its concentration is
tracer (Pant et al., 2000) but no data is available for its use in measured as a function of time at the outlet, then E(t)
waterkerosene environment. Therefore, validation of radiotracer representing the probability for a tracer element to have a
was carried out by thoroughly mixing about 0.1 mCi 99mTc in equal residence time between the time interval (t, t+dt) is dened as
amounts of water and kerosene. Upon separation and measure-
C t
ments, the radiotracer was found suitable for labeling water phase Ei t R 1 i (4)
in waterkerosene environment. About 0.5 mCi of 99mTc eluted 0 C i t dt

from a 99Mo/99mTc generator was injected in the form of an such that

instantaneous pulse to carry out RTD experiments for investiga- Z 1
tion of the hydrodynamics of dispersed phase (water) as per Ei t dt 1 (5)
experimental plan shown in Fig. 1. The experiments were carried 0

out for a range of pulsation frequency and amplitude as given in where i 1,2,3,y,n, Ci(t) is the tracer concentration, Ei(t) is the
Table 1. The movement of radiotracer was monitored for every RTD function.
second with the help of lead collimated 2 in  2 in NaI(Tl) RTD models have been playing a vital role for industrial
scintillation detectors mounted at D1, D2 and D3 as shown in process investigations from decades. They provide macroscopic
Fig. 1. The data was acquired on-line using a multi-channel data lumped sum description, which is sufcient for many engineering
acquisition system and stored in a computer for processing. calculations. The plug ow is an ideal condition for the ow of
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Ghiyas Ud Din et al. / Applied Radiation and Isotopes 67 (2009) 12481253 1251

phases in an extraction column but some degree of axial mixing is The ow conditions are not plug type before and after the inlet
always inevitable. The pulsation and closely spaced sieve plates (D2) and outlet (D3) boundaries, therefore, openopen boundary
inside the column continues to re-arrange the droplets of the condition can be chosen in present situation. A uniform radial
dispersed phase randomly. Keeping in view of these considera- concentration in the dispersed phase is assumed due to large
tions, the ADM was used to study the system hydrodynamics. length to diameter ratio.
The basic general differential equation of the one dimensional
ADM for uid ow in the dimensionless form is as follows:
0.03
Ud x 100 = 0.34 m/s @C 1 @2 C @C
Uc x 100 = 0.37 m/s  (6)
0.025 A x 100 = 1 m @y Pe @X 2 @X
input (D2) f = 0.95 s-1
where C is the dimensionless tracer concentration c(t)/c(0), Pe is
0.02
the Peclet number uL/D, X is the dimensionless axial coor-
dinate x/L, u is the mean linear velocity, D is the axial dispersion
E (t)

0.015 coefcient, c(t) is the tracer concentration at time t, and c(0) is the
initial tracer concentration. A detailed analysis and solution of Eq.
0.01 (6) have been given in (Levenspiel and Smith, 1957; Levenspiel,
Model output
Experimental output (D3)
1999).
0.005 A RTD analysis software package RTD developed by IAEA
(2004) was used for modeling in the present investigations. Two
0 point measurements methodology has been adopted for this
0 100 200 300 400 500 600 700 800 model in this software package. Fig. 2 shows typical normalized
Time (s) RTD curves obtained at the input (D2) and output (D3) with model
Fig. 2. Typical normalized RTD curves at the input (D2) and output (D3) with
output response of the dispersed phase in the pulsed sieve plate
model output response of dispersed phase in the pulsed sieve plate extraction extraction column in response to an instantaneous pulse injection
column. at (D1).

200 100 45
Ud x 100 Uc x 100 A x 100
190 90 (m/s) (m/s) (m) 40
180 0.34 0.37 1.00
80
Experimental MRT (s)

0.44 0.47 1.00 35

170
Peclet Number

Peclet Number
70
160 30
60
150 25
50
140
20
130 Ud x 100 Uc x 100 A x 100 40
(m/s) (m/s) (m)
30 15
120 0.34 0.37 1.00
0.44 0.47 1.00
110 20 10
0.5 0.7 0.9 1.1 1.3 1.5 1.7 1.9 2.1 0.6 0.8 1 1.2 1.4 1.6 1.8 2
Pulsation frequency (s-1) Pulsation frequency (s-1)

2.20
0.39 Ud x 100 Uc x 100 A x 100
2.10 (m/s) (m/s) (m)
0.37 0.34 0.37 1.00
2.00
Dispersed phase holdup

0.44 0.47 1.00

Slip velocity (m/s)

0.35
1.90
0.33 1.80
0.31 1.70
Ud x 100 Uc x 100 A x 100
0.29 (m/s) (m/s) (m)
1.60
0.34 0.37 1.00 1.50
0.27
0.44 0.47 1.00

0.25 1.40
0.5 0.7 0.9 1.1 1.3 1.5 1.7 1.9 2.1 0.5 0.7 0.9 1.1 1.3 1.5 1.7 1.9 2.1
Pulsation frequency (s ) -1 Pulsation frequency (s-1)

Fig. 3. (a) Effect of pulsation frequency on the MRT of dispersed phase; (b) effect of pulsation frequency on the Peclet number of the dispersed phase; (c) effect of pulsation
frequency on the dispersed phase holdup; (d) effect of pulsation frequency on the slip velocity of dispersed phase.
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1252 Ghiyas Ud Din et al. / Applied Radiation and Isotopes 67 (2009) 12481253

a b
36 60
215 Ud x 100 Uc x 100 f
34 (m/s) (m/s) (s-1) 55
195 0.34 0.37 1.12
32 50
Experimental MRT (s)

0.44 0.47 1.12

175

Peclet Number
Peclet Number
30 45
155
28 40
135
26 35
115 Ud x 100 Uc x 100 f
(m/s) (m/s) (s-1) 24 30
95 0.34 0.37 1.12
0.44 0.47 1.12 22 25

75 20 20
0.7 0.9 1.1 1.3 1.5 1.7 0.7 0.9 1.1 1.3 1.5 1.7
Pulsation amplitude x 100 (m) Pulsation amplitude x 100 (m)
c d
0.49 2.30
2.20 Ud x 100 Uc x 100 f
(m/s) (m/s) (s-1)
0.44 2.10 0.34 0.37 1.12
Dispersed phase holdup

0.44 0.47 1.12

2.00
Slip velocity (m/s)

0.39 1.90
1.80
0.34 1.70

Ud x 100 Uc x 100 f 1.60

(m/s) (m/s) (s-1)
0.29 1.50
0.34 0.37 1.12
0.44 0.47 1.12 1.40
0.24 1.30
0.7 0.9 1.1 1.3 1.5 1.7 0.7 0.9 1.1 1.3 1.5 1.7
Pulsation amplitude x 100 (m) Pulsation amplitude x 100 (m)

Fig. 4. (a) Effect of pulsation amplitude on the MRT of dispersed phase; (b) effect of pulsation amplitude on the Peclet number of the dispersed phase; (c) effect of pulsation
amplitude on the dispersed phase holdup; (d) effect of pulsation amplitude on the slip velocity of the dispersed phase.

3. Results and discussion 250

230
Model Mean Residence Time (s)

Fig. 3(ad) shows the effect of pulsation frequency on the MRT,

210
axial mixing, holdup and slip velocity of the dispersed phase for
two constant sets of Uc, Ud and pulsation amplitude. It has been 190
observed that increase in pulsation frequency increases the MRT 170
of dispersed phase until it approaches a maximum asymptotic 150
value. A similar trend in the axial mixing of the dispersed phase
130
has been observed as Peclet number decreases with increase
in pulsation frequency and then approaches a minimum value 110
Fig. 3(b). The increasing trend of MRT of dispersed phase is 90
qualitatively in agreement with those of Srinikethan et al. (1987) 70
who have carried out this kind of investigations on a 15 cm
50
diameter reciprocating plate column using sodium chloride
50 70 90 110 130 150 170 190 210 230 250
solution as tracer and conductivity cell as detector. However, an
Experimental Mean Residence Time (s)
asymptotic trend in MRT of the dispersed phase after achieving a
maximum value has been seen in present investigations by Fig. 5. Comparison of experimental and model MRTs.
covering a wider range of operating conditions. In fact, increase
in pulsation frequency increases the droplet population density
inside the column leading to an increase in dispersed phase present scenario as can be seen from Eq. (2). The slip velocity of
holdup. This phenomenon continues till a maximum holdup is dispersed phase decreases with increase in pulsation frequency
reached corresponding to a minimum drop size obtainable under until a minimum value is obtained beyond which no decrease has
the available operating conditions. At this stage, the column is been observed as can be seen from Fig. 3(d). This is due to the fact
densely packed with droplets and no further droplets can be that increase in droplet population density with increase in
accommodated Fig. 3(c). Similar is the reason for the behavior pulsation frequency leads to the situation where velocity elds
of MRT curve as it is directly proportional to the holdup in the around the droplets interferes with each other. Also, decrease in
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Ghiyas Ud Din et al. / Applied Radiation and Isotopes 67 (2009) 12481253 1253

the size of a droplet increases the drag on this droplet and hence Pakistan Institute of Engineering and Applied Sciences [PIEAS] is
decreases its velocity to move counter currently through the thankfully acknowledged.
continuous phase. The slip velocity of dispersed phase remains
decreasing till a minimum drop size has been obtained under the References
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The authors are grateful to the Higher Education Commission radiotracers and radioisotope sealed sources-II. Faculty of Mechanical
[HEC] for nancial support in accomplishment of this study. The Engineering, Department of Process Engineering, Praha, CTU.
authors are greatly indebted to the International Atomic Energy Thyn, J., Zitny, R., Kluson, J., Cechak, T., 2000. Analysis and diagnostics of industrial
processes by radiotracers and radioisotope sealed sources-I. Faculty of
Agency (IAEA) for providing RTD analysis software package. The
Mechanical Engineering, Department of Process Engineering, Praha, CTU.
cooperation and technical assistance extended by Pakistan Venkatanarasaiah, D., Varma, Y.B.G., 1998. Dispersed phase holdup and mass
Institute of Nuclear Science and Technology [PINSTECH] and transfer in liquid pulsed column. Bioprocess Eng. 18 (2), 119126.