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Abstract  

Dispersion number is a direct indication of the settling and coalescing property of solvent with the given aqueous system. By dispersion number measurement, suitability of solvent can be characterized for post-mixing settling operations during solvent extraction. Tri-isoamyl phosphate (TiAP) is being proposed as extractant, alternate to conventional extractant TBP for nuclear solvent extraction processes. In this work, TiAP is characterized by measuring the dispersion numbers for 36% TiAP in n-dodecane and 100% TiAP solutions, equilibrated with aqueous nitric acid solutions of varying concentrations.

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Abstract  

Formation and thermal decomposition of red-oil during unit operations of nuclear fuel cycle process flowsheets is a severe risk. In the literature, red-oil formation has been investigated thoroughly in general and in detail after Tomsk-7 incident on 6th April 1993. However there is no information on the thermal decomposition of formed red-oil. In this work, results of unique experiments on adiabatic thermal decomposition of red-oil, red-oil equilibrated with excess of 4N nitric acid and 100% TBP equilibrated with excess of 4N nitric acid have been discussed.

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Abstract  

Accidental exposure dose assessment by electron spin resonance (ESR) technique from the free radicals generated in a cotton handkerchief has been attempted in this investigation. The cotton handkerchief, a common material carried by individuals, was taken as the medium for free radical estimation. About 55 mg of the irradiated piece of cloth was loaded into a quartz tube and the dose dependence of the ESR signal at g=2.0026 was measured at room temperature, using a Bruker ESP-300 ESR spectrometer in X-band (9.74 GHz). The intensity of this signal was found to be proportional to the dose in the range of 1–1000 Gy. The stability of the free radicals with time of storage was followed. Dependence of dose rate as well as the presence of water on the yield of free radicals were also investigated.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Deepak Dicholkar
,
Lalit Patil
,
Vilas Gaikar
,
Shekhar Kumar
,
U. Kamachi Mudali
, and
R. Natarajan

Abstract  

The high performance liquid chromatography and gas chromatography methods were investigated for their applicability in determining micro-level concentrations of tri-n-butyl phosphate (TBP). A high performance liquid chromatograph (HPLC) equipped with refractive index detector was used in determining TBP up to 2 ppm concentration level in the aqueous nitric acid solutions. The gas chromatography incorporated with Thermionic Detector (NPD) and Flame Photometric Detector (FPD) were examined for their potential in analyzing TBP in organic phase up to sub-ppm level. The results indicated that HPLC-RI technique is well suited for direct analysis of aqueous phase. For organic phase analysis, gas chromatographic methods with the TID and FPD were suitable but performance of detectors deteriorated often due to fouling.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Shekhar Kumar
,
Bijendra Kumar
,
M. Sampath
,
D. Sivakumar
,
U. Kamachi Mudali
, and
R. Natarajan

Abstract  

Nuclear solvent extraction was traditionally performed with packed columns, pulse columns, mixer-settlers and centrifugal extractors. However for rapid separations at micro-flow level, micro mixer-settlers were desired and in the past, few of them were actually designed and operated in nuclear solvent extraction research. In the current era of micro-reactor and microchannel devices, there is a renewed interest for micro-mixer-settlers for costly solvents and specialty solutes where small flow-rate is not an issue. In this article, development of a simple but effective micro-mixer-settler for nuclear solvent extraction is reported. The developed unit was tested with 30% TBP/n-dodecane/nitric acid system and in both the regimes of mass transfer c → d (mass transfer from continuous phase to dispersed phase, also written as c → d) and d → c (mass transfer from dispersed phase to continuous phase, also written as d → c) nearly 100% efficiency was observed in extraction as well as stripping modes of operation.

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Abstract  

A spectrophotometric method is developed for the determination of dissolved tri-n butyl phosphate (TBP) in aqueous streams of Purex process used in nuclear fuel reprocessing. The method is based on the formation of phosphomolybdate with added ammonium molybdate followed by reduction with hydrazine sulphate in acid medium. Orthophosphate and molybdate ions combine in acidic solution to give molybdophosphoric (phosphomolybdic) acid, which upon selective reduction (with hydrazinium sulphate) produces a blue colour, due to molybdenum blue. The intensity of blue colour is proportional to the amount of phosphate. If the acidity at the time of reduction is 0.5 M in sulphuric acid and hydrazinium sulphate is the reductant, the resulting blue complex exhibits maximum absorption at 810–840 nm. The system obeys Lambert–Beer’s law at 830 nm in the concentration range of 0.1–1.0 μg/ml of phosphate. Molar Absorptivity was determined to be 3.1 × 10L mol−1 cm−1 at 830 nm. The results obtained are reproducible with standard deviation of 1 % and relative error less than 2 % and are in good agreement with those obtained by ion chromatographic technique.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Shekhar Kumar
,
S. Balasubramonian
,
Pranay Sinha
,
D. Sivakumar
,
U. Kamachi Mudali
, and
R. Natarajan

Abstract  

Thermophysical properties of reversed TALSPEAK extractant (0.3 M D2EPHA/0.2 M TBP/n-dodecane) were not available in literature. Authors have experimentally measured and correlated several thermophysical properties of RT solvent like density, viscosity, refractive index, acid uptake and flash point. In this paper, results of these studies will be discussed in detail.

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Abstract  

Supercritical CO2 assisted dissolution of metals and metal-oxides and in situ extraction by TBP (or co-solvent) has been reported in literature. However, in this work, the dissolution and in situ extraction by nitric acid solvates of TBP and alternate solvent TiAP has been reported for g-level UO2 (essentially PHWR fuel pellet fragments) feeds at atmospheric pressure without requiring supercritical fluids. Encouraging results were obtained.

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Abstract  

Recently authors demonstrated direct dissolution of g-level PHWR UO2 fuel pellet fragments and in situ extraction by TBP-HNO3 and TiAP-HNO3 solutions at atmospheric pressures. Extending the work, similar studies were performed on intact unirradiated PHWR UO2 fuel pellets (~15 g U) with varying compositions of organic solvate of tri-n-butyl phosphate (TBP). It was observed that extent of dissolution was a strong function of organic solution composition TBP·(HNO3) x (H2O) y . Complete dissolution of intact UO2 pellet in a reasonable time was observed only in case of a particular solvate composition.

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Abstract  

The tail-end purification of Am from Pu loading effluents in 7.5M HNO3 containing 160 mg l–1 Am and 1.2 mg l–1 Pu has been carried out. With 0.2M CMPO+1.2M TBP in dodecane as the extractant and stripping by 0.04M HNO3+0.05M NaNO2, the Pu level is brought down to 31.2 g l–1. When the acidity was reduced to 4.2M HNO3, one contact with 20% TLA/dodecane and subsequent extraction by a mixture of CMPO and TBP and stripping with 0.04M HNO3+0.05M NaNO2 gave Am samples without any detectable amounts of Pu. The recovery of Am was 90% by the first procedure and 98% by the second one.

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