期刊
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
卷 66, 期 5, 页码 394-398出版社
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.sab.2011.04.013
关键词
Microwave-assisted digestion; ICP OES; CVG-ICP-MS; Trace elements; Oxygen pressure
类别
资金
- Conselho Nacional de Desenvolvimento Cientifico e Tecnologico (CNPq)
- Instituto Nacional de Ciencia e Tecnologia de Bioanalitica [573672/2008-3]
- Instituto Nacional de Ciencias e Tecnologias Analiticas Avancadas [573894/2008-6]
- Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior (CAPES)
- Fundacao de Amparo a Pesquisa do Estado de Sao Paulo (FAPESP) [2006/59083-9]
The feasibility of using diluted HNO3 solutions under oxygen pressure for decomposition of whole and non-fat milk powders and whey powder samples has been evaluated. Digestion efficiency was evaluated by determining the carbon content in solution (digests) and the determination of Ca, Cd, Cu, Fe, K. Mg, Mn, Mo, Na, Pb and Zn was performed by inductively coupled plasma optical emission spectrometry and Hg by chemical vapor generation coupled to inductively coupled plasma mass spectrometry. Samples (up to 500 mg) were digested using HNO3 solutions (1 to 14 mol L-1) and the effect of oxygen pressure was evaluated between 2.5 and 20 bar. It was possible to perform the digestion of 500 mg of milk powder using 2 mol L-1 HNO3 with oxygen pressure ranging from 7.5 to 20 bar with resultant carbon content in digests lower than 1700 mg L-1. Using optimized conditions, less than 0.86 mL of concentrated nitric acid (14 mol L-1) was enough to digest 500 mg of sample. The accuracy was evaluated by determination of metal concentrations in certified reference materials, which presented an agreement better than 95% (Student's t test, P<0.05) for all the analytes. (C) 2011 Elsevier B.V. All rights reserved.
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