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Purification of americium from assorted analytical wastein hydrochloric acid medium
A. Sengupta • S. K. Thulasidas • V. C. Adya •
P. K. Mohapatra • S. V. Godbole • V. K. Manchanda
Received: 8 November 2011 / Published online: 23 November 2011
� Akademiai Kiado, Budapest, Hungary 2011
Abstract During the simultaneous extraction of plutonium
and uranium using anion exchange chromatographic technique
from analytical waste in hydrochloric acid medium, 241Am
which is invariably present in the plutonium bearing fuel
samples remains in the effluent. A two step separation scheme
was developed for the recovery and purification of Am from the
assorted waste to facilitate the disposal of large volume of
aqueous waste and the purified Am solution was utilized for
spectroscopic investigation. The separation scheme involved
solvent extraction using 0.1 M TODGA ? 0.5 M DHOA for
separation of americium from Fe, Pb, Ni and Na followed by
extraction chromatographic technique using CMPO on inert
support as stationary phase for separation of Ca from Am. A
systematic study on the extraction behavior of Am from
hydrochloric acid medium revealed that out of four extraction
systems well known for actinide partitioning namely 0.1 M
TODGA ? 0.5 M DHOA, 1 M DMDBTDMA, 0.2 M
CMPO ? 1.2 M TBP and 30% TRPO, only 0.1 M TOD-
GA ? 0.5 M DHOA extracts americium from 7.5 M HCl feed
acidity. A comparative study involving CMPO solvent
extraction and column chromatographic technique revealed
that elution of Am from column is satisfactory as compared to
inefficient stripping of Am from organic phase in solvent
extraction technique using 0.1 M HNO3. The purity of the final
solution was checked for 17 elements of interest and was found
to be 98% pure, while the overall recovery of this two step
separation scheme was found to be 95%.
Keywords Americium � TODGA � DHOA � CMPO �DMDBTDMA � TRPO � Analytical waste
Introduction
Due to high specific activity of 241Am, which is invariably
present in plutonium bearing fuel samples, the large volume of
effluent waste generated during the simultaneous extraction of
Pu and U on anion exchange column from analytical waste in
hydrochloric acid medium, could not be disposed off. Am
which is rich in emission spectra was found to interfere during
the analysis of trace constituents in plutonium based fuel
samples by ICP-AES based method involving separation of
Pu using 30% TBP-CCl4 followed by the analysis of raffinate
for trace constituents. 241Am also has wide applications as a
low energy gamma source because of its cost, convenience,
spectral purity and half-life [1, 2]. The major use of 241Am
is in smoke detector alarms and as radiography source [1, 3].
It is also used as a target material for the production of244Cm, 252Cf and higher transuranic elements and is
particularly useful for a wide range of industrial gauging
applications and as source of alpha radiation. 241Am-Be and a
large number of such sources are worldwide used in oil-well
logging operations [1, 3]. Therefore an attempt was made for
the recovery and purification of americium from the assorted
analytical waste to facilitate the disposal of waste and to use
purified americium for spectroscopic and other applications.
In aged Pu samples, the growth of 241Am activity is due to
the decay of 241Pu. Typically about 50 mg of 241Am is gen-
erated from about 1 g of 241Pu per year whose content in Pu
sample depends on the burn-up of the fuel and its storage time.
A. Sengupta (&) � S. K. Thulasidas � V. C. Adya �P. K. Mohapatra � S. V. Godbole
Radiochemistry Division, Bhabha Atomic Research Centre,
Trombay, India
e-mail: [email protected]
V. K. Manchanda
Department of Energy Science, Sungkyunkwan University,
Suwon 440-746, Republic of Korea
123
J Radioanal Nucl Chem (2012) 292:1017–1023
DOI 10.1007/s10967-011-1554-4
Attempts were made for recovery and purification of ameri-
cium from different kinds of waste generated either during
reprocessing of spent fuels or analytical waste generated
during quality control programme [4–6]. Separation of
americium from waste, soil, sediments and bio assay samples
using different extractants involving solvent extraction and
extraction chromatographic techniques followed by its esti-
mation have been reported in literature [7–15]. An overview
on great number of analytical methods for the determination
of 241Am isotope in environmental and nuclear samples
involving alpha and gamma spectrometry; liquid scintillation
technique and mass spectrometry was reported by Vajda et al.
[16]. Earlier we have reported a methodology for separation
and purification of americium from nitric acid medium and its
characterization by instrumental neutron activation analysis
[4, 17]. The present work involved development of an ana-
lytical methodology for purification of 22 mg of americium
from analytical waste in hydrochloric acid medium containing
130 mg of Ca, 32 mg of Pb, 24 mg of Ni, 33 mg of Fe and
133 mg of Na as major constituents. It was observed that to
extract americium from hydrochloric acid medium, 0.1 M
TODGA ? 0.5 M DHOA is effective from 7.5 M feed
acidity. Systematic study revealed that Pb, Ni, Fe and Na can
be separated from americium in hydrochloric acid feed using
solvent extraction with 0.1 M TODGA ? 0.5 M DHOA as
organic phase while Ca can be separated using column chro-
matographic technique with CMPO as stationary phase. The
purity of final americium solution was found to be *98%
while the overall recovery of the two step separation scheme
involving solvent extraction and extraction chromatography
was found to be 95%.
Experimental
Reagents
TODGA and DHOA were synthesized by previously reported
methods and their purities were determined by 1H MR, ele-
mental analysis and distribution coefficient measurements of
Am3? and UO22? respectively [18, 19]. Octylphenyl-N,
N-diisobutyl carbamoylmethyl phosphine oxide (CMPO)
and N,N0-dimethyl-N,N0-dibutyltetradecylmalonamide
(DMDBTDMA) were synthesized by reported method and
their purity was checked by their distribution behaviour
towards Am3? [20–22]. The CMPO loaded resin was pre-
pared by a method reported earlier [22]. Suprapure grade
nitric acid (Merck, Germany) was used throughout this work
and spec pure chemicals were used for making the elemental
standard solutions for ICP-AES analysis. n-dodecane was
procured from Koch-Light Laboratories, USA and Lancas-
ter, UK, respectively. The TBP solution (30% in n-dodecane)
was washed with 5% Na2CO3 to remove acidic impurities.
Methods
Extraction behavior of Am(III) using TODGA, CMPO,
DMDBTDMA and TRPO from hydrochloric acid medium
Since there was no literature available to the best of our
knowledge, to compare the extraction behavior of Am from
hydrochloric acid feed using extractants well known for
actinide partitioning, a systematic study of DAm values
versus the acidity (HCl(M)) of the aqueous feed was car-
ried out using 241Am tracer to optimize the extraction of
americium from hydrochloric acid using four extractants
namely 0.1 M TODGA ? 0.5 M DHOA, 1 M
DMDBTDMA, 0.2 M CMPO ? 1.2 M TBP and 30%
TRPO.
Extraction behavior of Fe(III), Ca(II), Pb(II), Ni(II),
Na(I) from hydrochloric acid medium using TODGA
ICP-AES analysis revealed that Fe, Ca, Pb. Ni and Na are
the major constituents of the waste along with americium.
With the aim of separation of americium from these ele-
ments by means of the extraction of americium in organic
phase leaving the impurities in the raffinate, studies were
carried out to understand the extraction behavior of these
elements from hydrochloric acid medium using 0.1 M
TODGA ? 0.5 M DHOA in dodecane as organic phase
which was found to be the best for extraction of americium
from hydrochloric acid feed. 1mg/mL concentration of
each element was allowed to equilibrate with the organic
phase for 2 h and the raffinate was analyzed for the ele-
ments mentioned above by ICP-AES.
Comparative study of CMPO solvent extraction
and CMPO column extraction
Above study revealed that americium cannot be separated
from calcium using TODGA from hydrochloric acid medium.
To get optimum condition a comparative study between sol-
vent extraction using CMPO as organic phase and column
chromatography using CMPO as stationary phase was carried
out. A feed containing 6.235 mg of Am in 150 mL having
3.5 M HNO3 acidity was equilibrated with equal volume of
organic phase (0.2 M CMPO ? 1.2 M TBP) for 1 h. After
complete phase separation, both the phases were analyzed
radiometrically,
The feed solution containing 6.097 mg of Am, at an acidity
of *3.5 M HNO3 in 115 mL was used for CMPO column
chromatographic extraction experiment. The feed solution
was loaded on the column with a rate of 2–3 drops per minute
after preconditioning with 50 mL of 3.5 M HNO3. The loaded
column was then washed thoroughly using 50 mL of 3.5 M
HNO3, so that the loosely bound or trapped ions were washed
1018 A. Sengupta et al.
123
out leaving Am?3 loaded on the column. Subsequently after
washing, Am3? held on the column was eluted using 0.01 M
HNO3 solution with a flow rate of 2–3 drops per minutes with
50 mL batches and was analyzed radiometrically.
Behavior of Ca(II) through CMPO column
The uptake and extraction behavior of Ca(II) was needed to
be investigated using CMPO column to confirm the com-
plete removal of Ca from the solution of our interest. Using
different concentrations of Ca (184–1,840 lg/mL) with a
feed acidity 3.5 M HNO3, the chromatographic extraction
studies were carried out using CMPO column precondi-
tioned with 25 mL of 3.5 M HNO3. The concentration
range for Ca(II) was chosen such that the concentration of
Ca(II) in the solution of our interest (Ca—867 lg/mL) was
within that range. Effluent, washing solution and eluant
were analyzed for Ca using ICP-AES technique.
Separation of Fe(III), Pb(II), Ni(II)
and Na(I) from americium
Based on the above studies, the waste solution containing
130 mg of Ca, 32 mg of Pb, 24 mg of Ni, 33 mg of Fe and
133 mg of Na as major constituents along with 22 mg of Am
was subjected to solvent extraction using 0.1 M TOD-
GA ? 0.5 M DHOA as organic phase for separation of Fe,
Pb, Ni and Na from Am. Two contacts of organic phase with
a:o =1:1 were used for complete extraction of Am leaving Fe,
Pb, Ni and Na in the raffinate. Subsequently the loaded organic
phase was stripped back using three contacts of pH-2 (0.01 M
HNO3). Mass distribution of americium in different fractions
generated was determined radiometrically while the impurity
analysis was carried out using ICP-AES.
Separation of Ca(II) from americium
CMPO column chromatographic technique using 5 g of TRU-
Spec CMPO resin material with a column (10 9 1 cm) of
10 mL bed volume was used for removal of Ca(II). The
specifications of CMPO column are given in Table 1. The
strip solutions from the TODGA step were mixed together and
the acidity was adjusted to 3 M HNO3 by adding suitable
amounts of supra pure HNO3 acid solution. To avoid break-
through of the column, the feed was divided into two equal
volumes and was passed through the column (which was
preconditioned with 3.5 M HNO3) with a rate of 4–5 drops per
minute. After loading, the column was washed with 5 bed
volumes of 3.5 M HNO3 and subsequently Am was eluted
using 0.01 M of HNO3 solution. Mass distribution of ameri-
cium was determined using radiometry while ICP-AES was
used for determination of impurities in the different fractions
obtained during the step.
Instruments
Radiometric estimation was used for determination of
americium in different fractions using 300 9 300 NaI (Tl)
well type scintillator detector. A suitable aliquot of each
sample was counted for sufficient time to get around
10,000 counts to restrict statistical counting error.
Impurity analyses were carried out using JY-Ultima
high resolution ICP-AES having practical resolution of
\0.005nm and has a continuous coverage of spectral range
200–800 nm. The specifications and working conditions of
the spectrometer are summarized in Table 2.
Results and discussions
Extraction behavior of Am(III) using TODGA, CMPO,
DMDBTDMA and TRPO from hydrochloric acid
medium
Figure 1 represents the extraction profiles of americium using
four promising extractants known for actinide partitioning
Table 1 Specification of CMPO extraction chromatography column
Parameters Specifications
Stationary phase 0.2 M CMPO ? 1.2 M TBP
Supported materials Chromosorb W
Mesh size (micron) 100–150
Amounts of resin in the column 5 g
Column length 10 cm
Bed volume 10 mL
Table 2 Specifications and operating conditions of JY-ULTIMA-
HR-ICP-AES
Optical design 1 M Czerny Turner
Grating Holographic, ion etched optical grating
Groove density 2,400 grooves/mm
Grating size 110 9 110 mm
Wave length range 120–800 nm
Band pass 0.0023 nm from 120–340 nm
0.0046 nm from 340–800 nm
Thermal regulation Controlled to 30±1 �C
RF generator
Frequency 40.68 MHz
Oscillator 27.12 MHz
Pump Dual channel (12 roller)
Nebulizer Pneumatic concentric
Operating condition
Ar plasma flow 13 L/min
Integration time 10 s
Reflected power \10 W
Sample flow rate 1 mL/min
Purification of americium from assorted 1019
123
(TODGA, CMPO, DMDBTDMA and TRPO) at various
hydrochloric feed acidity. It was found that there was practi-
cally no extraction of americium from hydrochloric acid
medium using 30% TRPO in dodecane throughout the
observed acidity range. The similar observation was found to
be true in case of 1 M DMDBTDMA in dodecane system also
while a steady increase in DAm was found beyond 6 M HCl in
case of 0.2 M CMPO ? 1.2 M TBP system. In case of 0.1 M
TODGA ? 0.5 M DHOA in dodecane system it was
observed that there was a steady increase in DAm up to 7 M
feed acidity and subsequently it attained a maxima with
DAm = 23 (% extraction = 95 with A:O = 1:1) followed by
decrease in DAm value. It was found that for effective
extraction of americium from hydrochloric acid medium
0.1 M TODGA ? 0.5 M DHOA in dodecane as organic
phase and 7.5 M feed acidity is required.
Extraction behavior of Fe(III), Ca(II), Pb(II), Ni(II),
Na(I) from hydrochloric acid medium using TODGA
On the basis of above study TODGA was found to extract
americium from HCl medium. With the aim to extract amer-
icium leaving behind the impurities in the raffinate, a sys-
tematic study was carried out to understand the extraction
behavior of the major constituents of the waste using TODGA
at varying HCl feed acidity (Fig. 2). It was found that there
was practically no extraction of Na, Fe, Ni and Pb throughout
the acidity range while in case of Ca, there was a sharp
increase in DCa value up to 6 M HCl and subsequently after
obtaining a maxima, decrease in DCa value was observed. The
extraction profile of Ca suggested that at 7.5 M feed acidity
*70% Ca would be coextracted along with americium. The
study revealed that, though 0.1 M TODGA ? 0.5 M DHOA
in dodecane system was found to effective for separation of
americium from Na, Fe, Ni and Pb, additional separation step
was necessary for separation of Ca.
Comparative study of CMPO solvent extraction
and CMPO column extraction
With the aim of extraction of americium from Ca, a
comparative study involving solvent extraction and
extraction chromatographic technique using CMPO as
extractant was carried out which suggested that 91% of the
feed (*5.5 mg of Am) was extracted in the organic phase
after one contact. Subsequently the loaded organic phase
was back extracted using pH *2 solution with A:O = 2:1.
Radiometric determination revealed that after one contact,
only 28% of the loaded Am could be stripped back sug-
gesting pH *2 solution is not effective for back extraction
of loaded americium. However, 0.4 M formic
acid ? 0.4 M hydrazine hydrate ? 0.1 M citric acid mix-
ture was effective for quantitative back extraction of Am.
Since the tubing of ICP-AES instrument was made up of
organic polymer, stripping of Am using organic complex-
ing agents does not conform to ICP-AES analysis. Am
distribution in different fractions is summarized in Table 3.
In case of extraction chromatographic technique, major
amount of the loaded Am was eluted in the first fraction.
*57% of the feed Am i.e. 3.505 mg was eluted in first
50 mL fraction. In other three fractions the amounts of Am
eluted out were 18.5, 6, 4 lg respectively in each 50 mL
0 1 2 3 4 5 6 7 8 9 10
0
5
10
15
20
25
DA
m
HCl(M)
30% TRPO
0.1M TODGA+0.5M DHOA
0.2M CMPO+1.2M TBP
1M DMDBTDMA
Fig. 1 Extraction behavior of Am(III) using TODGA, CMPO,
DMDBTDMA and TRPO from hydrochloric acid medium
2 4 6 8 10
0.01
0.1
1
10
D
HCl (M)
Ca
Na
Ni
Fe
Pb
Fig. 2 Extraction behavior of Ca(III), Fe(II), Ni(II), Na(I), Pb(II)
using 0.1 M TODGA ? 0.5 M DHOA from hydrochloric acid
medium
1020 A. Sengupta et al.
123
(Table 4). The amount of Am present in the fourth fraction
indicated that almost all loaded Am was eluted out in four
fractions. From this comparative study it can be concluded
that CMPO column with proper capacity could be used for
Am3? uptake and quantitative elution by 0.01 M HNO3.
Behavior of Ca(II) through CMPO column
With the aim of loading americium on the CMPO column
leaving Ca in the effluent, behavior of Ca through CMPO
column was studied. These studies revealed that in the
above concentration range Ca(II) was not held on CMPO
column and the effluent was found to contain major amount
of Ca. There was some amount of Ca which was trapped in
the column bed but it could subsequently be washed out
using five bed volumes of 3.5 M HNO3 solution (Table 5).
These experiments suggested that CMPO column is
effective for separation of Ca from americium.
Purification of americium from the waste
On the basis of above preliminary studies, two contacts of
0.1 M TODGA ? 0.5 M DHOA in dodecane with
A:O = 1:1 were given to the waste solution whose feed
was adjusted to 7.5 M HCl for quantitative separation of
americium from Pb, Ni, Na and Fe. The organic phase
which was loaded with americium along with Ca was
subsequently stripped by three contacts of 0.01 M HNO3.
82% of americium was stripped in first contact while the
overall recovery of this separation step was found to be
more than 99%. The decontamination factors for Pb, Ni, Fe
and Na were found to be 640000, 480000, 660000 and
2660000 respectively while that of Ca was found to be 1.1.
All the strip solutions were mixed together and the acidity
was adjusted to 3.5 M HNO3 for making proper feed of
CMPO column chromatographic extraction. Mass distri-
bution of americium at various fractions generated in this
step is summarized in Table 6.
To avoid the breakthrough of the column, the separated
solution was divided into two equal volumes and loaded on
the CMPO column maintaining the flow rate mentioned
earlier. Americium was found to be quantitatively held on
the column as suggested by the radiometric estimation of
americium in the raffinate. The loaded column was sub-
sequently washed thoroughly with 50 mL of 3.5 M HNO3
followed by elution with 0.01 M HNO3 in three batches of
total 150 mL volume. The first fraction was found to
contain 99% of americium while quantitative elution was
confirmed by estimation of americium in the third fraction.
Similar process was followed for the second feed for
CMPO extraction after preconditioning the column with
3.5 M HNO3. Table 7 represents the mass distribution of
americium at different fractions generated in CMPO step.
The overall recovery of this step was found to be 98%
while the decontamination factor for Ca was 24,00,000.
ICP-AES was employed for determination of impurity in
the solutions generated after each separation step with 10%
RSD (Table 8). The purity of the final purified americium
solution was checked for the analytes of interest using the
interference free analytical channels identified in our previous
Table 3 Am distribution in different fractions generated during
CMPO solvent extraction
Fractions Amount of
Am (mg)
Volume
(mL)
%
Recovery
Feed for CMPO solvent
extraction (aqueous phase
acidity 3.5 M HNO3)
6.235 150 –
Aq. phase after extraction 0.565 150 9
Org. phase after stripping 3.812 150 61
Strip solution (pH 2) 1.610 300 26
Table 4 Extraction and elution behavior of Am(III) using
TRU-SPEC� CMPO column
Fractions Amount of
Am (mg)
Volume
(mL)
% Recovery
Feed for CMPO column 6.0972 115 –
Effluent 0.976 115 16
Washing solution 1.525 50 25
Eluant-1 3.505 50 58
Eluant-2 0.019 50 0.3
Eluant-3 0.006 50 0.1
Eluant-4 0.004 50 0.06
Table 5 Extraction behavior of Ca(II) using CMPO column
Fractions
(lg/mL)
Preconditioning
(lg/mL)
Effluent
(lg/mL)
Washing
solution
(lg/mL)
Eluant
(lg/mL)
184 BDL 170 11.90 BDL
368 BDL 341 24.90 BDL
920 BDL 846 59.25 BDL
1840 BDL 1727 142.50 BDL
Table 6 Mass distributions of Am(III) at different fractions gener-
ated during TODGA-DHOA extraction in HCl medium
Fractions Volume (mL) Am(mg) % Recovery
Am stock 150 22.7 ± 0.7 –
Loaded TODGA 300 22.6 ± 0.6 99.56
Depleted aqueous 150 0.04 ± 0.001 0.17
Strip 1 50 18.6 ± 0.2 81.94
Strip 2 50 3.2 ± 0.3 14.10
Strip 3 50 0.87 ± 0.09 3.80
Purification of americium from assorted 1021
123
study [23]. The final solution was found to be 98% pure as
mentioned in Table 9 while the overall recovery of this two
step separation scheme was found to be 95%.
Conclusions
In conclusion it can be highlighted that a two step sepa-
ration scheme involving solvent extraction and extraction
chromatography was developed for purification of milli-
gram quantities of americium from the analytical waste in
hydrochloric acid medium containing Ca, Fe, Na, Ni, Pb as
major constituents (Fig. 3). TODGA was used for separa-
tion of americium from Pb, Ni, Fe and Na with decon-
tamination factors 640000, 480000, 660000 and 2660000
respectively while Ca can be separated using CMPO col-
umn chromatography with D.F. 2400000. The final solu-
tion was found to be 98% pure with respect to 17 analytes
of interest while the overall recovery of these two step
separation scheme was 95%. This work is optimization and
demonstration of the methodology for purification of mil-
ligram amounts of americium from assorted waste in
hydrochloric acid medium.
Table 7 Mass distribution of Am(III) in different fractions generated during CMPO step
Fractions Part-1 % Recovery Part-2 % Recovery
Am Volume (mL) Am Volume (mL)
Feed for CMPO 10.9 ± 0.7 100 – 11.0 ± 0.7 100 –
Effluent 0.08 ± 0.005 lg 100 0.73 0.03 ± 0.005 lg 100 0.27
Washing 0.04 ± 0.005 lg 50 0.37 0.03 ± 0.004 lg 50 0.27
Eluant-1 10.8 ± 0.4 mg 50 99.08 10.7 ± 0.6 mg 50 97.27
Eluant-2 8 ± 0.6 lg 50 0.07 5 ± 0.4 lg 50 0.04
Eluant-3 BDL 50 – BDL 50 –
Table 8 ICP-AES analysis of different fractions generated during
Am purification from HCl medium
Elements Am-stock
(mg)
TODGA strip
(mg)
CMPO eluant
(mg)
Ca 130 ± 5 120 ± 5 BDL
Pb 32 ± 3 BDL BDL
Ni 24 ± 2 BDL BDL
Fe 33 ± 3 BDL BDL
Na 133 ± 3 BDL BDL
Table 9 Determination of trace
elements in purified Am (Am—
100 lg/mL) by ICP-AES
Elements Conc in Am
matrix (lg/mL)
Eu \0.05
Dy \0.05
Gd 2
Sm \0.05
Fe \0.05
Ca \0.05
Na \0.05
Cr \0.05
Ag \0.05
Al \0.05
Co \0.05
Mn \0.05
Mg \0.05
Ni \0.05
Cd \0.05
Zn \0.05
Cu \0.05
Analytical waste (Am, Fe, Pb, Ni, Na, Ca)
7.5M HCl feed
Separation of Fe, Pb, Ni and Na from americium:
1. Extraction with 0.1M TODGA + 0.5M DHOA from 7.5M HCl 2. Stripping with 0.01M HNO3
Separation of Ca from americium:
1. Feed was adjusted to 3.5M HNO3 and loaded on CMPO column 2. After washing with 5 bed volumes of 3.5M HNO3, elution with
0.01M HNO3
Purified americium solution
Purity – 98%, Overall recovery – 95%
Fig. 3 Proposed flow sheet of purification of americium from
analytical waste in hydrochloric acid medium
1022 A. Sengupta et al.
123
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