Abstract
Mobilisation of alpha emitting radionuclides from silicious base sample is one the challenging task for environmental radiochemist. During this study, rapid and complete dissolution of the siliceous base samples were carried out by optimizing temperature, pressure and power of the microwaves. The Pu-239+240 in digested samples was pre-concentrated by scavenging Fe as Fe(OH)3. Pu-239+240 was isolated from the Fe(OH)3 by co-precipitating Pu with Bi(PO4) in HNO3 medium at pH 2. Pu-239+240 was separated from Bi(PO4) and other transuranics by passing through cation and anion exchange resin. Pu-239+240 was counted by alpha spectrometry after electroplating on stainless steel planchet. The detection limits achieved for Pu-239+240 was 60 μBq/g (2.6 × 10−14 g/g). Pu-242 was used as a tracer for the evaluation of recovery of Pu-239+240. Samples prepared after complete destruction of matrix in microwave, showed 10–20% higher concentration of Pu-239+240 compared to conventional acid leached. Consistent recovery in the range of 97–99% for Pu-242 were observed in microwave digested samples whereas inconsistent results were observed in acid leached samples where the recoveries were in the range of 75–86%. Siliceous matrix degradation was tracked by monitoring the surface morphology and composition of the residue left at various stages of digestion using Scanning Electron Microscope (SEM) coupled with Energy dispersive X-ray spectrometer (EDS).
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