Abstract
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.
Highlights
Kingston and Jassie[1] and Kingston and Haswell[2] have published landmark books that demonstrated the benefits of microwave radiation for sample digestion and for enhancing chemical processes in several areas of science
This study evaluated three vessel designs for digestions of rice flour and bovine liver samples using dilute nitric acid solutions
This section was structured to describe the analytical performance of each rotor and respective vessels starting from the simplest one, MAXI 44, followed by SK-15 vessels, and, for the single reaction chamber technology (SRC) technology
Summary
Kingston and Jassie[1] and Kingston and Haswell[2] have published landmark books that demonstrated the benefits of microwave radiation for sample digestion and for enhancing chemical processes in several areas of science. Krug and Rocha[3] and Flores[4] have edited books that demonstrated how this technology has evolved and nowadays it is broadly applied. In this context, microwaveassisted digestion has progressively become a standard procedure for sample preparation and it has clear impact in procedures applied for trace analysis and green chemistry.[5]. It became clear that microwave radiation is an alternative for fast heating of solutions containing ions and dipoles, but it is a strategy for implementing better and more effective analytical procedures. The use of dilute nitric acid solutions for performing digestions represents a step forward in the
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