A new sorbent, thorium oxalate incorporated in silica gel matrix was prepared. This material was characterized by X-ray, Thermo-gravimetric
Analysis, surface area and porosity analysis. The material was obtained in the form of granular particles in the mesh size
range of 80–150 American Standard of Testing Materials, yielding good liquid flow, when packed in ion exchange column. This
sorbent was investigated for the sorption of americium from various aqueous media such as nitric acid, oxalic acid and sulphuric
acid by distribution coefficient studies. Column experiments were carried out to study the practical application of this sorbent
for removal of americium from oxalic acid-nitric acid solutions. Elution studies were also carried out for the recovery of
Authors:R. Bhanushali, I. Pius, S. Mukerjee, and V. Vaidya
As a part of treatment of low level active waste, co-precipitation of plutonium (Pu) and americium (Am), with thorium oxalate,
from oxalate supernatants generated during plutonium oxalate precipitation has been investigated. A simple method for the
simultaneous removal of both Pu and Am from oxalate supernatants could be developed. This simple process achieves incorporation
of these alpha active nuclides into small volumes of solid matrix from large volumes of aqueous waste.
Authors:I. Pius, R. Bhanushali, K. Pillai, S. Mukerjee, and V. Vaidya
Sorption of Pu(IV) on alumina microspheres prepared by the sol-gel procedure has been investigated for the recovery of plutonium
from nitric acid-oxalic acid solutions. Distribution ratio for Pu(IV) between alumina microspheres and nitric acid-oxalic
acid have been determined. The influence of the mode of preparation and heat treatment of these microspheres, on the sorption
of Pu(IV) have been investigated. Pu(IV) breakthrough capacities have been determined using a 5 ml bed of alumina with solutions
of Pu(IV) in 1M HNO3+0.05M H2C2O4 and 0.5M HNO3+0.05M H2C2O4. The elution behavior of Pu(IV) loaded on these microspheres were studied using nitric acid solutions containing different
oxidising and reducing agents. Investigations were also carried out to fix the activity in the alumina matrix by heat treatment.
Authors:I. Pius, M. Charyulu, C. Sivaramakrishnan, and S. Patil
Distribution ratios of Pu(IV) between 7.5M HNO3+0.75M H3PO4+0.3M H2SO4 media and a macroporous anion-exchange resin Amberlyst A-26 (MP) increased from 40 to 250 when 1M aluminium nitrate was added to the aqueous medium. When 1M ferric nitrate was used in place of aluminium nitrate the distribution ratio further increased to 850. The 10% Pu(IV) breakthrough capacities with a 5 ml bed resin column, using synthetic feed solutions containing 1M aluminium nitrate, were 1.4 g l–1, 3.2 g l–1 at flow rates of 30 ml per hour and 10 ml per hour, respectively. The corresponding 10% Pu(IV) breakthrough capacities in the presence of 1M ferric nitrate were 8.5 g l–1 and 12.8 g l–1. More than 97% of plutonium could be recovered from actual analytical phosphate waste solutions.
Authors:I. Pius, M. Charyulu, C. Sivaramakrishnan, and S. Patil
The extraction of Pu(IV) from oxalic acid-nitric acid mixtures has been investigated using a liquid anion exchanger, Aliquat-336, in xylene. The presence of oxalic acid is known to have adverse effects on the extraction of Pu(IV) by Aliquat-336. The use of cations, Al(III), Fe(III) or Zr(IV) was explored to overcome the effect of oxalic acid on Pu(IV) extraction. The data obtained reveal that Pu(IV) is quantitatively extracted by Aliquat-336, even in the presence of oxalic acid, when Al(III), Fe(III) or Zr(IV) is added. The extracted Pu(IV) can be back-extracted using aqueous ammonium carbonate.
Authors:R. Bhanushali, I. Pius, S. Mukherjee, and V. Vaidya
A new ion exchange material prepared by impregnating Aliquat-336 on silica-gel has been investigated for the recovery of plutonium from nitric-oxalic acid solutions. The distribution ratio of Pu(IV) was studied at various concentrations of nitric and oxalic acids. The presence of Al(III) and Fe(III) in the solution, enhances the uptake of Pu(IV). Pu(IV) breakthrough capacities (btc) have been determined using 2.5 ml bed of the ion exchange material column in the absence and the presence of Al(III) and Fe(III) nitrate. The elution behavior of Pu(IV) was also studied using nitric acid solutions containing reducing agents. More than 90% of plutonium could be recovered from nitric-oxalic acid solutions.
Authors:I. Pius, M. Charyulu, B. Venkataramani, C. Sivaramakrishnan, and S. Patil
Sorption of Pu(IV) from sodium carbonate medium has been investigated by using three inorganic ion exchangers, viz. alumina, silica gel and hydrous titanium oxide (HTO). Distribution ratios (D) of Pu(IV) for its sorption on these ion exchangers have been determined. The values are 700, 103 and 104 for alumina, silica gel and hydrous titanium oxide, respectively, from 0.1M sodium carbonate medium. The high distribution ratios indicate their suitability for the removal of Pu(IV) from sodium carbonate waste streams. Pu(IV) breakthrough capacities have been determined with 5 ml bed at a flow rate of 30 ml per hour. The 10% Pu(IV) breakthough capacities for alumina and silica gel are 3 g l–1 and 14 g l–1, respectively. The capacity of HTO is 60 g of Pu(IV) per liter of exchanger at 4% Pu(IV) breakthrough.
Authors:I. Pius, Aruna Kadam, M. Rao, V. Rao, and P. Natarajan
Results of experiments on the adsorption of plutonium (IV) on alumina and their application to the recovery of plutonium from analytical waste solutions containing phosphoric-nitric acid are reported. Distribution ratios of plutonium (IV) between alumina and solutions containing varying concentrations of phosphoric acid and nitric acid are determined. The influence of various ions like UO22+, Fe3+, MoO42–, VO2+ and SO42– on the distribution ratio is evaluated. Saturation values of adsorption of plutonium (IV) on alumina and optimum conditions for loading and elution of plutonium on a column packed with alumina are described.
Authors:V. Rao, I. Pius, M. Subbarao, A. Chinnusamy, and P. Natarajan
A method for the precipitation of plutonium(IV) oxalate from homogeneous solutions using diethyl oxalate is reported. The precipitate obtained is crystalline and easily filterable with yields in the range of 92–98% for precipitations involving a few mg to g quantities of plutonium. Decontamination factors for common impurities such as U(VI), Am(III) and Fe(III) were determined. TGA and chemical analysis of the compound indicate its composition as Pu(C2O4)2·6H2O. Data are obtained on the solubility of the oxalate in nitric acid and in mixtures of nitric acid and oxalic acid of varying concentrations. Green PuO2 obtained by calcination of the oxalate has specifications within the recommended values for trace foreign substances such as chlorine, fluorine, carbon and nitrogen.