Waste minimization through high-pressure microwave digestion of soils for gross α/β analyses

As a result of the U.S. Department of Energy's (DOE) environmental restoration and waste management activities, laboratories receive numerous analytical requests for gross α/β analyses. Traditional sample preparation methods for gross α/β analysis of environmental and mixed waste samples require repetitive leaching, which is time consuming and generates large volumes of secondary wastes. An alternative to leaching is microwave digestion. In the past. microwave technology has had limited application in the radiochemical laboratory because of restrictions on sample size resulting from vessel pressure limitations. However, new microwave vessel designs allow for pressures on the order of 11 MPa (1500 psi). A procedure is described in which microwave digestion is used to prepare environmental soil samples for gross α/β analysis. Results indicate that the described procedure meets performance requirements for several soil types and is equivalent to traditional digestion techniques. No statistical differences at the 95% confidence interval exist between the measurement on samples prepared from the hot plate and microwave digestion procedures for those soils tested. Moreover, microwave digestion allows samples to be prepared in a fraction of the time with significantly less acid and with lower potential of cross-contamination. In comparison to the traditional hot plate method, the waste volumes required for the microwave procedure are a factor of 10 lower, while the analyst time for sample processing is at least a factor of three lower