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Preparation of Food Samples Using Homogenization and Microwave-Assisted Wet Acid Digestion for Multi-Element Determination with ICP-MS
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Focused microwave-induced combustion: a new technique for sample digestion.

Márcia F Mesko1, Juliana S F Pereira, Diogo P Moraes

  • 1Instituto de Química e Geociências, Universidade Federal de Pelotas, 96010-610, Pelotas, RS, Brazil.

Analytical Chemistry
|February 11, 2010
PubMed
Summary

A novel focused microwave-induced combustion (FMIC) procedure efficiently digests botanical samples for elemental analysis. This method offers complete decomposition with minimal reagents, enabling lower detection limits for trace elements.

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Area of Science:

  • Analytical Chemistry
  • Environmental Science

Background:

  • Traditional sample digestion methods can be time-consuming and require large amounts of reagents.
  • Accurate elemental analysis is crucial for environmental monitoring and material science.

Purpose of the Study:

  • To develop and evaluate a rapid sample digestion procedure using focused microwave-induced combustion (FMIC).
  • To assess the efficiency of FMIC for the determination of multiple elements in botanical samples.

Main Methods:

  • Development of an FMIC system using a modified microwave oven and quartz sample holder.
  • Combustion of pelletized botanical samples with oxygen flow and ammonium nitrate igniter.
  • Optimization of parameters including reflux step, sample mass, and combustion time.
  • Elemental analysis using inductively coupled plasma optical emission spectrometry (ICP-OES).

Main Results:

  • Complete sample decomposition (residual carbon <0.5%) achieved in under 2 minutes at temperatures >950°C.
  • High agreement (95-103%) with certified reference materials using FMIC with a reflux step.
  • Low reagent consumption (10 mL diluted nitric acid) and low relative standard deviation (<3.8%).
  • Ability to digest large sample masses (up to 1500 mg), leading to lower detection limits.

Conclusions:

  • FMIC is a rapid, efficient, and reagent-sparing technique for botanical sample digestion.
  • The developed FMIC procedure is suitable for trace element determination by ICP-OES.
  • This method offers advantages over conventional microwave-assisted digestion techniques.