Abstract
A procedure is described by which plutonium and americium can be determined in environmental samples. The sample is leached with nitric acid and hydrogen peroxide, and the two elements are co-precipitated with ferric hydroxide and calcium oxalate. The calcium oxalate is incinerated at 450° and the ash is dissolved in nitric acid. Plutonium is extracted with tri-n-octylamine solution in xylene from 4 M nitric acid and stripped with ammonium iodide/hydrochloric acid. Americium is extracted with thenoyltrifluoroacetone solution in xylene at pH 4 together with rare-earth elements and stripped with 1 M nitric acid. Americium and the rare-earth elements thus separated are sorbed on Dowex 1 × 4 resin from 1 M nitric acid in 93% methanol, the rare-earth elements are eluted with 0.1 M hydrochloric acid/0.5 M ammonium thiocyanate/80% methanol and the americium is finally eluted with 1.5 M hydrochloric acid in 86% methanol. Plutonium and americium in each fraction are electro-deposited and determined by alpha-spectrometry. Overall average recoveries are 81% for plutonium and 59% for americium.
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