Radiochemical Determination of Plutonium-239 in Low-Level Environmental Samples by Electrodeposition

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Abstract
Aqueous solutions of known plutonium content and a variety of environmental media to which a known amount of plutonium was added were assayed by a scheme of chemical analysis including electrodeposition of plutonium on stainless steel planchets for alpha counting. The method is particularly effective in the range of n-to-pc (10−9–10−12 c) per mg to 10 g amounts of sample solids such as soil, silt, food ash, rain, etc. Depending on precision desired the samples are prepared for analysis by one of three general methods-wet combustion and acid leaching (HNO3) of up to 10 g sample solids, sodium peroxide sintering of up to 0.5 g sample solids, or sodium carbonate fusion of up to 1 g sample solids. The solubilized plutonium as the chloride is reduced to the trivalent state, coprecipitated with lanthanum carrier as the fluoride, dissolved in acid aluminum nitrate and extracted with thenoyltrifluoracetone (TTA) for separation and removal of impurities and carrier. The plutonium is then back-extracted with strong acid, oxidized and electrodeposited on stainless steel for counting. The yield for these “weightless samples” is estimated at over 83 per cent for samples containing in the order of 1–10 pc of plutonium per sample and over 95 per cent for larger amounts of plutonium.

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