A chemical separation procedure is described which allows the direct determination of low241Pu activities in environmental samples with a windowless gas-flow proportional counter. While current separation schemes based on anion exchange yield counting sources of sufficient purity for subsequent α-spectrometry, for β-counting of241Pu additional purification steps are required. A combination of anion exchange from 9 mol/l HCl, LaF3 precipitation and TTA extraction was found to be suitable even for the analysis of long-range Chernobyl fallout samples which contained interfering radionuclides with β-activities at least 3 to 4 orders of magnitude higher than usually encountered. No difference is detectable between the results of the present, direct procedure and the results of the conventional indirect method based on the build-up of241Am. Average241Pu/239+240Pu ratios in air and deposition samples taken at Neuherberg near Munich were 70±6 with the present procedure and 66±9 from241Am build-up.
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