Microwave-Assisted Acid Digestion: Evaluation of Reaction Vessel Design and Performance

Nowadays, microwave-assisted procedures using closed vessels with thermal, chemical, and mechanical resistance are the state-of-the-art for efficient digestion of samples. Safety issues related to sample reactivity should be considered and analytical throughput is also a critical parameter. The choice of a specific vessel for a target application is not trivial and simple experiments are presented here for rice flour and bovine liver samples to illustrate effects of vessel design on digestion performance. Despite using the same heating program, the residual carbon contents varied from 22 to 67% to bovine liver digests and from 7 to 96% to rice flour digests. Quantitative recoveries were obtained for most analytes. Low recoveries were observed mainly for Ca and Fe. Analytical performance is related to different sizes, shapes and the gradient of temperature for each model of digestion vessel. It was demonstrated that taller vessels improved regeneration of nitric acid.

Keywords:
microwave radiation; sample preparation; closed vessel; digestion efficiency; ICP OES