Microwave-assisted digestion of organic samples: How simple can it become?

  • Nóbrega J
  • Pirola C
  • Fialho L
 et al. 
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Abstract

Advancements in sample preparation for performing trace analysis of inorganic analytes are coming from the dissemination of microwave-assisted procedures, but there is still room for improvements by looking for simple and easily applied procedures. Recently it was proposed a new approach called single reaction chamber with capability for digestions at high pressures and temperatures using simple vials and racks. This was a limitation of former cavity microwave ovens with closed vessels. It was demonstrated here that the use of single reaction chamber approach allows the implementation of efficient digestions using diluted solutions of nitric acid and also allows addressing a critical need of sample preparation for inorganic analysis by running mixed batches of samples. The feasibility of this procedure was demonstrated for organic samples and accuracy was proved by using certified reference materials of apple leaves, bovine liver and whole milk powder. Digestions performed of whole milk powder and bovine liver using 2.0 mol L-1nitric acid solution plus concentrated hydrogen peroxide at 240°C led to residual carbon contents of 0.825 and 1.50% and residual acidities of 1.04 and 0.618 mol L-1, respectively. These parameters are fully compatible with further measurements using ICP OES or ICP-MS. Al, Cu, Fe, Mn, Mo, Rb, Se, Sr, and Zn were accurately determined by ICP OES or ICP-MS depending on their concentrations in digests. © 2012 Elsevier B.V. All rights reserved.

Author-supplied keywords

  • Diluted nitric acid solutions
  • Microwave-assisted digestion
  • Residual Acidity
  • Residual Carbon
  • Single reaction chamber
  • Temperature of digestion

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Authors

  • J. A. Nóbrega

  • C. Pirola

  • L. L. Fialho

  • G. Rota

  • C. E.K.M.A. De Campos Jordão

  • F. Pollo

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