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This work was performed as part of a broader effort to automate analytical methods for determination of plutonium and other radioisotopes in environmental samples. The work described here represented a screening study to determine the potential for applying ultrasonic irradiation to sample digestion. Two standard reference materials (SRMs) were used in this study: Columbia River Sediment and Rocky Flats Soil. The key experiments performed are listed below along with a summary of the results. The action of nitric acid, regardless of its concentration and liquid-to-solid ratio, did not achieve dissolution efficiency better that 20%. The major fraction of natural organic matter (NOM) remained undissolved by this treatment. Sonication did not result in improved dissolution for the SRMs tested. The action of hydrofluoric acid at concentrations of 8 M and higher achieved much more pronounced dissolution (up to 97% dissolved for the Rocky Flats soil sample and up to 78% dissolved for the Columbia River Sediment sample). Dissolution efficiency remains constant for solid-to-liquid ratios of up to 0.05 to 1 and decreases for the higher loadings of the solid phase. Sonication produced no measurable effect in improving the dissolution of the samples compared with the control digestion experiments. Combined treatment of the SRM by mixtures of HNO3 and HF showed inferior performance compared with the HF alone. An adverse effect of sonication was found for the Rocky Flats soil material, which became more noticeable at higher HF concentrations. Sonication of the Columbia River sediment samples had no positive effect in the mixed acid treatment. The results indicate that applying ultrasound in an isolated cup horn configuration does not offer any advantage over conventional ''heat and mix'' treatment for dissolution of the soil and sediment based on the SRM examined here. This conclusion, however, is based on an approach that uses gravimetric analysis to determine gross dissolution efficiency. This approach does not allow any conclusion regarding the possible advantage of sonication in selective dissolution of plutonium traces incorporated into an inorganic or organic fraction of the samples

Sonochemical Digestion of Soil and Sediment Samples