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Updated: Jun 28, 2026

Preparation of Food Samples Using Homogenization and Microwave-Assisted Wet Acid Digestion for Multi-Element Determination with ICP-MS
Published on: December 22, 2023
Determination of volatile elements in biological materials by isotopic dilution ETV-ICP-MS after dissolution with
D Pozebon1, V L Dressler, A J Curtius
1Departamento de Quimica da Universidade Federal de Santa Catarina, Campus Universitario Trinidade, 88040-900 Florianópolis, S.C. Brazil.
Abstract:
Isotopic dilution for the determination of Ag, Cd, Hg, Pb and Tl in biological materials by ETV-ICP-MS is proposed. The sample was simply dissolved with tetramethylammonium hydroxide (TMAH) or acid digested in a microwave furnace, with an on line matrix separation. When the dissolution was employed, Ir was used as a chemical modifier for Hg and Pb and Pd was used for Cd and Tl. No modifier was used for Ag. The pyrolysis temperatures were taken from pyrolysis temperature curves. The on line preconcentration was performed in a flow injection system with solenoid valves and was based on the analyte complexation with ammonium diethyldithiophosphate and sorption of the complexes on C(18) bonded to silica gel in a minicolumn. For the digested sample submitted to the analyte preconcentration procedure, a modifier, Ir, was only used for Hg. For the other analytes, since a low pyrolysis temperature, 300 degrees C, was employed, no modifier was added. The isotopic dilution calibration was applied to two certified materials, bovine liver and dog fish muscle, dissolved with TMAH or acid digested, and to another two certified materials, corn bran and rice flour, acid digested and submitted to analyte preconcentration. The obtained concentration values agree with the certified ones, showing that this calibration procedure leads to accurate results in the determination of low concentrations of volatile elements. Due to simplicity, the dissolution with TMAH is very attractive.
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