Rapid method for the analysis of plutonium isotopes in a soil sample within 60 min.

A rapid method for the determination of Pu isotopes in a soil sample within 60 min of starting sample pretreatment was developed. The large reduction in the analysis time was attained by the rapid and perfect digestion of the sample using an alkaline fusion method with an induction heating machine. Pu concentrations were then determined by flow injection/ICP-MS using a solid extraction resin after preconcentration by batch extraction with a chelate resin. The limits of detection for 239Pu and 240Pu were 9.2 fg and 4.3 fg, corresponding to 0.03 and 0.05 Bq kg(-1), respectively, under our analytical conditions, which satisfy the lower detection limits (0.5 Bq kg(-1) of 239Pu, and 2 Bq kg(-1) of 240Pu) required for rapid analysis techniques by the Ministry of Education, Culture, Sports, Science and Technology, Japan. This method provides a powerful and practical technique for emergency monitoring in and around nuclear facilities that handle large amounts of plutonium.

Development of rapid plutonium analysis for environmental samples by isotope dilution/inductively coupled plasma mass spectrometry with on-line column.

This paper describes our development of a rapid on-line column/ID-ICP-MS technique for the analysis of plutonium (Pu) in environmental samples using an UTEVA extraction chromatograph resin (UTEVA resin) column. It took only 40 min to separate and measure Pu in the sample solution, including the time for conditioning the resin column for the next analysis. In our method, Pu in a 3 M nitric acid solution was fed to the UTEVA resin, and then eluted from the resin by reducing Pu to Pu(III) with 3 M nitric acid mixed with 0.01 M ascorbic acid after washing the resin. The outflow from the resin column was directly introduced to an ICP-MS system. The low concentration of ascorbic acid and the small volume of the eluting solution (0.6 mL) made successive stable analysis possible without any skimmer cone clogging. The chemical recovery of Pu during column operation was 70%, and typical lower detection limits for 239Pu, 240Pu and 242Pu were 9.2, 4.3 and 7.5 fg (21, 36 and 1.1 microBq), respectively. We analyzed five international standard materials for Pu, and obtained good results.