Use of microwave-assisted evaporation for the complete recovery of volatile species of inorganic trace analytes
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.
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DD
Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, Pennsylvania 15282-1503, USA.
Kingston
HM