Effect of simultaneous cooling on microwave-assisted wet digestion of biological samples with diluted nitric acid and O2 pressure |
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Authors: | Cezar A Bizzi Joaquim A Nóbrega Juliano S Barin Jussiane SS Oliveira Lucas Schmidt Paola A Mello Erico MM Flores |
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Institution: | 1. Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, Rio Grande do Sul 97105-900, Brazil;2. Departamento de Química, Universidade Federal de São Carlos, São Carlos, São Paulo 13565-905, Brazil;3. Departamento de Tecnologia e Ciência dos Alimentos, Universidade Federal de Santa Maria, Santa Maria, Rio Grande do Sul 97105-900, Brazil |
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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 (60–190 m3 h−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 (190 m3 h−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 190 m3 h−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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Keywords: | Microwave-assisted digestion Pressurized vessel Wet ashing Digestion efficiency Simultaneous cooling Mild conditions |
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