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Acid extraction and cloud point preconcentration as sample preparation strategies for cobalt determination in biological materials by thermospray flame furnace atomic absorption spectrometry
Authors:George L. Donati, Cl  sia C. Nascentes, Ana Rita A. Nogueira, Marco A.Z. Arruda,Joaquim A. N  brega
Affiliation:aGrupo de Análise Instrumental Aplicada, Departamento de Química, Universidade Federal de São Carlos, Caixa Postal 676, 13560-970, São Carlos, SP, Brazil;bDepartamento de Química, ICEx, Universidade Federal de Minas Gerais, Belo Horizonte, MG, Brazil;cEmbrapa Pecuária Sudeste, São Carlos, SP, Brazil;dInstituto de Química, Universidade Estadual de Campinas, Campinas, SP, Brazil
Abstract:A thermospray flame furnace atomic absorption spectrometer (TS-FF-AAS) was employed for Co determination in biological materials. Cobalt presents a high atomization temperature and consequently poor sensitivity is obtained without changing its thermochemical behavior. The effect of different complexing agents on sensitivity was evaluated based on the formation of Co volatile compounds. A cloud point procedure was optimized for Co preconcentration for further improvement of sensitivity. Samples were treated with 1 mol l− 1 hydrochloric acid solution for quantitative extraction of Co without simultaneous extraction of Fe, since it is a strong interferent. After the extraction and preconcentration steps, a sample volume of 150 μl was introduced into the hot Ni tube using air as carrier at a flow-rate of 0.4 ml min− 1. The best sensitivity was attained using ammonium pyrrolidinedithiocarbamate (APDC) and Triton X-114 was employed for implementation of the cloud point procedure. The detection limit obtained for Co was 2.1 μg l− 1 and the standard deviation was 5.8% for a solution containing 100 μg l− 1 (n = 10). Accuracy was checked using two certified reference materials (tomato leaves and bovine liver) and results were in agreement with certified values at a 95% confidence level. Employing the developed procedure, Co were quantified in different biological materials (plant and animal tissues). The proposed method presents suitable sensitivity for cobalt determination in the quality control of foods.
Keywords:Thermospray   Flame atomic absorption spectrometry   Tube in flame   Acid extraction   Cloud point extraction   Cobalt
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