Lemos Valfredo Azevedo, Baliza Patrícia Xavier, de Carvalho Anaildes Lago, Oliveira Rafael Vasconcelos, Teixeira Leonardo Sena Gomes, Bezerra Marcos Almeida
Universidade Estadual do Sudoeste da Bahia, Núcleo de Química Analítica da Bahia, Laboratório de Química Analítica, Campus de Jequié, 45.506-191 Jequié, Bahia, Brazil.
Talanta. 2008 Oct 19;77(1):388-93. doi: 10.1016/j.talanta.2008.06.046. Epub 2008 Jul 9.
A preconcentration method for manganese determination by sequential injection cloud point extraction with subsequent detection by flame atomic absorption spectrometry (FAAS) has been developed. The enrichment of Mn was performed after a preliminary on-line cloud point extraction and entrapment of manganese-containing surfactant aggregated within a minicolumn packed with cotton. The laboratory-made reagent 4-(5'-bromo-2'-thiazolylazo)orcinol (Br-TAO) and the surfactant Triton X-114 were used for cloud point extraction. The manganese ions were eluted with sulphuric acid solution and directly introduced into the FAAS. Chemical and flow variables affecting the preconcentration were studied. Using a sample volume of 2.80 mL the limit of detection and enrichment factor were calculated to be 0.5 microg L(-1) and 14, respectively. The sample frequency is 48 h(-1), considering a total run cycle of 75 s. The accuracy of the proposed method has been demonstrated by the analysis of the certified reference biological materials rice flour and tomato leaves. The method has been applied to determination of manganese in food samples.
建立了一种通过顺序注射浊点萃取预富集锰,随后采用火焰原子吸收光谱法(FAAS)进行检测的方法。在初步在线浊点萃取并将含锰表面活性剂聚集体截留在填充有棉花的微型柱内后,对锰进行富集。使用自制试剂4-(5'-溴-2'-噻唑基偶氮)邻苯二酚(Br-TAO)和表面活性剂Triton X-114进行浊点萃取。用硫酸溶液洗脱锰离子并直接引入FAAS中。研究了影响预富集的化学和流动变量。使用2.80 mL的样品体积时,计算得出检测限和富集因子分别为0.5 μg L⁻¹和14。考虑到总运行周期为75 s,样品频率为48 h⁻¹。通过对有证参考生物材料米粉和番茄叶进行分析,证明了该方法的准确性。该方法已应用于食品样品中锰的测定。