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Measurement of Aqueous Entrainment in the

Organic Product of 40 mm Dia DFRP Centrifugal
Extractor

Conference Paper · March 2014

DOI: 10.13140/2.1.3305.0402

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CHEMENT-2014 Contributed Paper
06-07 March 2014, Kalpakkam, India RD-01

Measurement of Aqueous Entrainment in the

Organic Product of 40 mm Dia DFRP Centrifugal Extractor
Shekhar Kumar*, Abhishek Singh, M. Balamurugan, U. Kamachi Mudali and R. Natarajan
Reprocessing R&D Division, Reprocessing Group, Indira Gandhi Centre for Atomic Research
Kalpakkam 603102.
*Corresponding author E-mail: shekhar@igcar.gov.in

Abstract
Water content in the organic phase product of 40mm dia DFRP centrifugal extractor was analyzed by Karlfisher
titration technique. Based on the base solubility value of water in the organic phase, the aqueous phase carryover in
the organic phase was estimated and was found to vary nearly linearly with O/A. In all the experimental conditions,
the entrainment was observed to be lower than flooding limit for centrifugal extractor.

Keywords: Centrifugal extractor, characterization, entrainment

device (Make: Toshiba). Aqueous and organic phases

Introduction
were fed by two valve-less pumps (ISMATEC Process
Stage type centrifugal extractors are unique type of
drive with FMI-Q3 head). Samples were taken after
mixer—settlers with small footprint [1]. Centrifugal
reaching the steady state which was checked by volume
extractor is the ideal choice of contactor for fast reactor
input–output balance.
fuel reprocessing operations where challenges of high
Pu concentration, low holdup and low residence time Karlfisher analysis was performed on a volumetric
are to be met. Since mixing in the annular zone of Karlfisher titrator (Metrohm-841KF) coupled with a
centrifugal extractor is often in the turbulent couette robotic 24-station autosamplechanger (814-USB).
zone due to excessive energy input, ultra small diameter Single component KF reagent (M/S Sigma-Aldrich,
droplets of dispersed phase are formed and due to equivalent to 5 mg/mL Water) was used. KF titrations
limitation of short residence time, their coalescence and were performed in dry methanol as non-aqueous media
capture is not complete. In this situation, a small The set up used for the experiments is shown in Fig.1.
carryover of dispersed phase is present in the continuous
phase. In case of continuous organic phase, higher
viscosity often results in poorer coalescence in the
setting zone. The related analysis is reported in
literature in detail [2-4]. Recently authors reported results
of studies of organic entrainment in the aqueous product
of the centrifugal extractor [5]. In this paper,
complementary results of studies on aqueous
entrainment in the organic phase are presented.
Experimental
Details of setup
The feed organic solution was prepared by diluting AR
grade TBP (Merck 99%+) with commercial n-dodecane
(~95%) to a final concentration of 30% (Vol.). The acid
solution (approx. 0.01 N) was prepared by diluting stock
acid (~15.6 N HNO3, Ranchem (69–72% w/w)) with
water. As aim of the experiments was to study primarily
hydrodynamics and related phenomena for the 40 mm Fig. 1 Water content in the organic samples being
dia centrifugal extractor, dilute acid (equivalent to analyzed by Automatic Robotic Karl Fischer titrator at
acidified water) was used. Since operations were RRDD
conducted in the operable zone having entrainment
much below the permissible limit of 1% (flooding Results and Discussion
The estimated water content of the organic phase is
limit), effect of acidity on the entrainment was
given in Table 1. At different O/A ratios, results
presumed to be not significant. The aqueous
indicate different values of water content for the same
entrainment in the organic phase was analyzed using
biphasic system of 30%TBP/nitric acid. The
Karl-Fisher titrator.
experimentally measured water content of organic phase
The 40 mm dia centrifugal extractor was similar to ANL has two components, a.the base solubility of water in
design having annular mixing zone. The equipment of the organic phase and b. phase carryover in the form of
in-house design was fabricated indigenously. Its rotor aqueous entrainment. The base solubility of water in
was coupled to a miniature 3 AC motor fed by a VFD 30% TBP/n-dodecane is taken as 8 gpl[6]. Based on this
 CHEMENT-2014 Contributed Paper
06-07 March 2014, Kalpakkam, India RD-01

value, the entrainment in the organic phase was methods. Based on the base solubility value of water in
estimated and given in Table 1. the organic phase, the aqueous phase carryover in the
organic phase was estimated and was found to vary
Table 1. Experimentally determined entrainment
nearly linearly with O/A. In all the experimental
values.
conditions, the entrainment was observed to be lower
Water Content Aqueous than the classical flooding limit for centrifugal extractor.
O/A ratio of Org Phase Entrainment
(g/kg) (%) References
1. G.S. Laddha and T.E. Degaleesan, Transport
0.1 6.46 ± 0.17 0.0006* Phenomena in Liquid Extraction, Tata McGraw
Hill, New Delhi, India, 1976.
0.5 8.21±0.62 0.2693
2. R. A. Leonard, G. J. Bernstein, A. A. Ziegler, and
1 8.83±0.05 0.3645 R. H. Pelto, Annular Centrifugal Contactors for
solvent extraction, Separation Science and
5 9.77±0.25 0.5089 Technology, 925–943 (1981)
10 11.67±3.50 0.8006 3. H. A. Arafat, M. C. Hash, A. S. Hebden, and R. A.
*Organic dispersed. Leonard, Characterization and recovery of solvent
entrained during the use of centrifugal contactors,
1 Tech. Rep. ANL-02/08, Argonne National
0.9
Laboratory, Argonne, Ill, USA, 2001.
0.8 4. B. Schuura, G. N. Kraaia, J. G. M. Winkelmana,
and H. J. Heeresa, Hydrodynamic features of
0.7
centrifugal contactor separators: experimental
Entrainment (%)

0.6 studies on liquid holdup, residence time

0.5 distribution, phase behavior and drop size
0.4
distributions, Chemical Engineering and
Processing, Vol. 55, 8–19 (2012).
0.3
5. Shekhar Kumar; R.S. Shekhawat; Abhishek Singh;
0.2
M. Balamurugan; N. Priyadarshini; M. Sampath; U.
0.1 Kamachi Mudali, Characterisation of submicron
0 -1 size entrainment in the aqueous product stream of a
0 1
10 10 10 40 mm diameter centrifugal extractor for 30%
O/A Phase ratio
TBP/nitric acid biphasic system, Int. J. of Nuclear
Fig.2. Variation of aqueous carryover with varying O/A
Energy Science and Technology, Vol.8, 49 – 60
phase ratio.
(2014)
The variation of aqueous carryover of the organic phase 6. Shekhar Kumar, Rajnish Kumar and S.B. Koganti,
could be expressed as a function of O/A ratio as shown An extended salt-effect model for organic solubility
in the Fig.2. This entrainment was less than the 1% of water in a 5-100% tri-n-butyl
entrainment limit for flooding. phosphate/diluent/nitric acid/water biphasic system
Conclusion at 298.15 K, Indian Journal of Chemical
Water content in the organic phase product of 40mm dia Technology, Vol.15, 287-290 (2008).
centrifugal extractor was analyzed by chemical

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