Santelli Ricardo Erthal, Bezerra Marcos de Almeida, de Santana Otoniel Domingos, Cassella Ricardo Jorgensen, Ferreira Sérgio Luis Costa
Universidade Federal Fluminense, Instituto de Química, Outeiro São João Batista, s/n Niterói, 24020-150 Rio de Janeiro, Brazil.
Talanta. 2006 Feb 15;68(4):1083-8. doi: 10.1016/j.talanta.2005.07.010.
This article describes the development by response surface methodology (RSM) of a procedure for iron, zinc and manganese determination by flame atomic absorption spectrometry (FAAS) in food samples after digestion employing a focussed microwave system. A Doehlert matrix was used to find optimal conditions for the procedure through response surface study. Three variables (irradiation power and time and composition of oxidant solution-HNO(3)+H(2)O(2)) were regarded as factors in the optimization study. The working conditions were established as a compromise between optimum values found for each analyte taking into consideration the robustness of the procedure. These values were 12min, 260W and 42% (v/v) for irradiation time, irradiation power and percent of H(2)O(2) in solution, respectively. The accuracy of the optimized procedure was evaluated by analysis of certified reference materials and by comparison with a well-established closed vessel microwave dissolution methodology.
本文介绍了采用聚焦微波系统消解食品样品后，通过响应面法（RSM）开发的一种火焰原子吸收光谱法（FAAS）测定铁、锌和锰的方法。采用Doehlert矩阵通过响应面研究来寻找该方法的最佳条件。在优化研究中，将三个变量（辐照功率、时间以及氧化溶液-HNO₃+H₂O₂的组成）视为因素。考虑到该方法的稳健性，将工作条件设定为每种分析物的最佳值之间的折衷。对于辐照时间、辐照功率和溶液中H₂O₂的百分比，这些值分别为12分钟、260瓦和42%（v/v）。通过分析有证标准物质并与成熟的密闭容器微波消解方法进行比较，评估了优化方法的准确性。
