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Abstracts  

Liquid–liquid extraction of gold(III) with two β-diketones e.g. Benzoyl acetone (BZAC) and theonyl trifluoro acetone (TTA) and enhancement effects of trioctyl phosphine oxide on such extractions in various organic media have been studied by radiotracer technique. Strong ternary adduct complex formation were reported in chloroform (BZAC chelate) and carbontetrachloride (TTA chelate) media. Effect of temperature variation established such processes as spontaneous, enthalpy favoured with net loss in entropy. Synergic effects were reported to be strongly diluent dependent and Hildebrand’s regular solution theory was found to be applicable in such systems.

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Abstract  

Rate constants for the reaction of the primary species of water radiolysis, viz. e aq' , H and OH, with picolinic acid have been determined at various pHs. The semi-reduced species exhibits max at 305 and 350 nm. It is a strong reductant and has two pKa values of 1 and 5.7. The OH adduct of this compound also exhibits two pKa s at 2.1 and 5.2. H-atom reaction with picolinic acid gives rise to a mixture of species.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: S. Tripathi, R. Kannan, P. Dhami, P. Naik, S. Munshi, P. Dey, N. Salvi, and S. Chattopadhyay

Abstract  

The improvement and the refinement of non-viable Rhizopus arrhizus biomass were investigated via immobilization. Immobilization was carried out by using sodium alginate/CaCl2 solution and formaldehyde/HCl cross-linking with dead Rhizopus arrhizus biomass and were used for the sorption of radionuclides from low level effluent wastes. The sodium alginate/CaCl2 immobilized biomass (ratio 1:2) showed about 86% sorption for 241Am activity but due to its soft nature and tendency to undergo distortion in shape, is unsuitable for practical applications. The biomass cross-linked with 15% formaldehyde/0.1 M HCl solution has a relatively high mechanical strength and rigidity. It was showing a sorption of >99% for 241Am activity and has the sorption capacity of ~65 mg/g for americium and uranium. Hence, it can be utilized for the removal of radionuclides from radioactive waste effluents.

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Abstract  

To achieve end user’s specified PuO2, controlling and monitoring of Pu in its fourth valency state is essential prior to the conversion of Pu-nitrate to its oxide through oxalate precipitation process. Conventional radiometric procedure for the analysis of Pu oxidation state in Pu-nitrate solution containing trace level of Pu(III) has limitation due to oxidation of Pu(III) during the sample preparation with respect to acidity. A simple direct spectrophotometry using an optic fiber spectrophotometer was attempted for the estimation of trace level of Pu(III), after separating the bulk amount of Pu(IV) by maintaining the sample acidity. By using a synergistic mixture of 30 % TBP and 1 M theonyl trifluoro acetone in benzene, the Pu(IV) could be removed to a level which doesn’t interfere in the Pu(III) absorption.

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Abstract  

During nuclear fuel reprocessing, monitoring of U and Pu concentration in every stage is very essential for process control purpose. A simple and fast spectrophotometric method for a simultaneous estimation of U and Pu in Plutonium Uranium Recovery by Extraction (PUREX) process’s tail end stream like Pu product where Pu concentration is much richer than that of U is described here. The method involves reduction of the bulk amount of Pu to Pu(III) using ascorbic acid in 1 M HNO3. Visible absorption peaks were measured at 416 nm for U and at 600 nm for Pu using a fiber optic probe of path length 40 mm. The methodology enables quantification of U and Pu concentration in the Pu product samples with a precision of 2.8 and 2.1%, respectively.

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Abstract  

Cross-linked hydrogel matrices immobilized with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HA), were prepared to investigate their application in the recovery of radionuclide from acidic waste solutions. Gamma-radiation was used to produce HA immobilized polyvinyl alcohol (PVA) hydrogels (HA-gel). The hydrogels with different characteristics such as: degree of cross-linking (by varying radiation dose) and quantity of extractant immobilized (by starting with aqueous PVA solution containing different amounts of HA), were synthesised. These HA-gels were investigated for solid-liquid phase extraction of U(VI), Pu(IV), Am(III) and some fission products, under various experimental conditions. The concentration of HNO3 in the aqueous phase was found to play an important role in the extraction of these radionuclei. Extraction of U(VI) was more favourable at lower concentration of HNO3 (∼0.001 to 0.5M), while at higher concentrations (∼0.5 to 3M HNO3), more than 90% of Pu(IV) present in the aqueous phase, could be extracted by the HA-gel. The extraction of Am(III) was also found predominant only at lower acidities (at pH∼2 and above). Under optimized conditions, maximum metal loading capacities obtained were 19±0.8 mg, 8±0.4 mg and 11±0.5 mg per gram of swollen HA-gel, for U(VI), Pu(IV) and Am(III), respectively. Under the experimental conditions, extractions of Cs(I) and Sr(II) were observed to be negligible. No leaching out of HA from the HA-gel particles was noted even after its repetitive use for the studied ten cycles of extraction and stripping experiments, as evident from its unchanged extraction efficiency.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: D. Pant, G. Chaugule, K. Gupta, P. Kulkarni, P. Gurba, P. Janardan, R. Changrani, P. Dey, P. Pathak, D. Prabhu, A. Kanekar, and V. Manchanda

Abstract  

This paper deals with the optimization of experimental conditions for the estimation of Np in spent fuel dissolver solution using 2-thenoyltrifluoroacetone (HTTA) as extractant. The quantitative extraction of Np from the dissolver solution employing 0.5 M HTTA/xylene was followed by its estimation by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) after stripping it from the organic phase with 8 M HNO3. The reliability of the method was checked by standard addition technique. The method is precise and accurate yielding Np analytical recovery of 99 ± 1%.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: S. Ravi, A. Deepa, B. Surekha, S. Susheela, P. Achuthan, S. Anil Kumar, K. Vijayan, U. Jambunathan, S. Munshi, and P. Dey

Abstract  

90Sr estimation in reprocessed uranium was carried out by a series of solvent extraction and carrier precipitation techniques using strontium and lanthanum carriers. Fuming with HClO4 was used to remove 106Ru as RuO4. Three step solvent extraction with 50% tri-n-butyl phosphate in xylene in presence of small amounts of dibutyl phosphate and thenoyl trifluoro acetone was carried out to eliminate uranium, plutonium, thorium and protactinium impurities. Lanthanum oxalate precipitation in acid medium was employed to scavenge the remaining multivalent ions. Strontium was precipitated as strontium oxalate in alkaline pH and 137 Cs was removed by washing the precipitate with water. A strontium recovery well above 70% was obtained. Final estimation was carried out by radiometry using end window GM counter after drying the precipitate under an infra red lamp. The same procedure was extended to the estimation of 90Sr in a diluted sample of the actual spent fuel solution. An additional lanthanum oxalate precipitation step was required to remove the entire 144Ce impurity from this sample. This modified procedure was employed in the determination of 90Sr in a number of reprocessed uranium samples and the over all precision of the method was found to be well within ±10%. An additional barium chromate precipitation step was necessary for the analysis of reprocessed uranium samples from high bumup fuels to eliminate trace amounts of short lived 224Ra produced during the decay of 232U and its daughters as they interfere in the estimation of 90Sr.

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