Determinação direta de constituintes inorganicos em leite por ICP OES : comparação critica do desempenho analitico em configuração de tocha axial e radial, usando uma mistura de animais terciarios (CFA-C) como solvente

AUTOR(ES)
DATA DE PUBLICAÇÃO

2004

RESUMO

In this work the insertion of milk samples in an instrument of optical emission in plasma (ICP OES) after a simple dilution in a mixture of soluble tertiary amines in water (CFA-C 10% v/v) was explored. Macro (Al, Ca, K, Mg, Na and P) and micro-elements (Al, Ba, Cu, Fe, Mn, Mo, Se and Zn) were determined using both plasma configurations axial and radial. The analytical performance of the ICP OES was evaluated considering the Mg II 280.2 nm / Mg I 285.2 nm ratio, matrix effects, BEC´s, SBR´s, LDO´s, LOQ´s, accuracy and precision. Using a nebulization gas-flow rate of 0.6 L min and applied power of 1.3 kW, the Mg II/Mg I was larger than eight for both configurations. Under robust conditions, the plasma processes were not changed significantly in the presence of 0.1% m/v of Ca, K or Na. This behavior was also observed for a series of analytical lines in a wide range of energy (1.6 - 15.9 eV), although effects up to 30 % have been observed for some lines (i.e. Al I 396 nm). Severe matrix effects were observed for the most analytical lines in non-robust conditions, mainly with AX-ICP OES. It was compensated by the use of Sc and Y as internal standards, mainly for AX-ICP OES under robust conditions, except for the Al I 396 nm atomic line (effects around 20 - 30 %). Although the determination of Al and Se was not possible, the accuracy of the results obtained (confidence interval of 98% for most of the analytical lines) in the presence of a complex matrix without the need of a previous digestion step, the quantification of commercial samples of milk proves the usefulness of this method developed for a fast and simple analysis of this kind of matrix.

ASSUNTO(S)

suspensão (quimica) quimica analitica leite produtos pereciveis

ACESSO AO ARTIGO

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