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Effect of simultaneous cooling on microwave-assisted wet digestion of biological samples with diluted nitric acid and O2 pressure

Analytica Chimica Acta
Publication Date
DOI: 10.1016/j.aca.2014.05.051
  • Microwave-Assisted Digestion
  • Pressurized Vessel
  • Wet Ashing
  • Digestion Efficiency
  • Simultaneous Cooling
  • Mild Conditions


Abstract The present work evaluates the influence of vessel cooling simultaneously to microwave-assisted digestion performed in a closed system with diluted HNO3 under O2 pressure. The effect of outside air flow-rates (60–190m3h−1) used for cooling of digestion vessels was evaluated. An improvement in digestion efficiency caused by the reduction of HNO3 partial pressure was observed when using higher air flow-rate (190m3h−1), decreasing the residual carbon content for whole milk powder from 21.7 to 9.3% (lowest and highest air flow-rate, respectively). The use of high air flow-rate outside the digestion vessel resulted in a higher temperature gradient between liquid and gas phases inside the digestion vessel and improved the efficiency of sample digestion. Since a more pronounced temperature gradient was obtained, it contributed for increasing the condensation rate and thus allowed a reduction in the HNO3 partial pressure of the digestion vessel, which improved the regeneration of HNO3. An air flow-rate of 190m3h−1 was selected for digestion of animal fat, bovine liver, ground soybean, non fat milk powder, oregano leaves, potato starch and whole milk powder samples, and a standard reference material of apple leaves (NIST 1515), bovine liver (NIST 1577) and whole milk powder (NIST 8435) for further metals determination by inductively coupled plasma atomic emission spectroscopy (ICP-OES). Results were in agreement with certified values and no interferences caused by matrix effects during the determination step were observed.

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