- Link: Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, Pennsylvania 15282-1503, USA.
Solutions must often be evaporated prior to analysis either to preconcentrate the analyte or to eliminate an incompatible matrix component. Elimination of the halogen-based acids HCI and HF using traditional evaporation methods poses recovery problems because of volatilization of the target analyte as the chloride or fluoride species. A new sample preparation chemistry for trace analysis, where losses of analyte due to volatilization during the evaporation process are minimized, is explored using the unique heating mechanisms of the microwave-assisted evaporation process. The heating mechanisms of hot plate evaporation and microwave-assisted evaporation are compared, and temperatures throughout the evaporation process using each method are predicted and experimentally verified. Because the solution actually cools during microwave-assisted evaporation, volatilization due to overheating at dryness is minimized. Elemental standard solutions and SRM soil and tissue digestates were evaporated using a hot plate method and a newly developed reduced-pressure microwave-assisted evaporation apparatus. Redissolution and analysis of the residue by ICPMS showed that complete recovery was achieved using microwave-assisted evaporation while losses of several classically volatile analytes occurred using hot plate evaporation.