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Singh G.,Advanced Fuel Fabrication Facility | Singhal R.K.,Advanced Fuel Fabrication Facility | Singhal R.K.,Bhabha Atomic Research Center | Malav R.K.,Advanced Fuel Fabrication Facility | And 4 more authors.
Analytical Methods | Year: 2011

ThO2 with approximately 3% 233UO2 is the proposed fuel for the Advanced Heavy Water Reactor (AHWR) and characterized as a mixed oxide (MOX) fuel. Due to the existence of a single oxidation state, quantitative dissolution of MOX samples like (Th-U)O2 and (Th-Pu)O2 is a challenging task for any analytical chemist. However, dissolution is a pre-requisite for complete characterization of the fuel. The present paper describes a detailed study carried out on the comparison of dissolution of sintered (Th-U)O2 mixed oxide pellets, in 16 M HNO3 using microwave and conventional heating techniques, under reflux conditions. The study was carried out with variation of parameters such as concentration of HF and UO2 substitution in the MOX solid solution. The concentration of dissolved U and Th was determined by modified Davies and Gray potentiometric titration and Th-EDTA complexometric titration using xylenol orange as the titration end point indicator respectively. Experimental results clearly indicate that the microwave heating assisted dissolution rate is 2 to 3 times higher than the conventional infrared heating assisted dissolution rate, for sintered pellets. The concentration of HF is a critical parameter, an excess leads to precipitation of insoluble ThF 4. The concentration of HF was optimized to 0.025 M. Experimental results also clearly show that at this concentration of HF in 16 M HNO 3, a higher substitution of UO2 in MOX solid solution also facilitates the dissolution process. Different trace metal impurities were determined in the MOX samples after dissolving by microwave and infra red heating techniques and it was observed that the results are comparable. © 2011 The Royal Society of Chemistry.

Somayajulu P.S.,Bhabha Atomic Research Center | Sengupta A.,Bhabha Atomic Research Center | Karande A.K.,Advanced Fuel Fabrication Facility | Malav R.,Advanced Fuel Fabrication Facility | And 2 more authors.
Journal of Radioanalytical and Nuclear Chemistry | Year: 2015

(Th,Pu)O2 fuel pellets were synthesised by coated agglomerate pelletization route and characterized for the chemical quality control. (Th,Pu)O2 pellets were characterized for trace metals by spectrometric methods and non metals by ion chromatographic, spectrophotometric, conductometric and manometric methods. H, F, B and Cd contents were found to be less than 1 ppm while that for V and Cl were found to be less than 10 ppm. The pellets were found to contain Cr, Cu, Mo, Na, Ni and Pb in the range of 10–50 ppm whereas Zn, Al, Ca and C in the range of 50–100 ppm. More than 100 ppm Si, Fe and Mg were found to be present in the (Th,Pu)O2 pellets. The O/M content of the pellets were found to be ~2.00. A comparative study on (Infrared) I.R. and microwave (microwave) dissolution were also used to ascertain the Th and Pu content in the (Th,Pu)O2 pellets. © 2015 Akadémiai Kiadó, Budapest, Hungary

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