Universidade Federal da Bahia, Instituto de Química, Programa de Pós-Graduação em Química, Campus Ondina, 40170-115, Salvador, Bahia, Brazil; Instituto Nacional de Ciência e Tecnologia de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, Bahia, Brazil.
Universidade Federal da Bahia, Instituto de Química, Programa de Pós-Graduação em Química, Campus Ondina, 40170-115, Salvador, Bahia, Brazil; Instituto Nacional de Ciência e Tecnologia de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, Bahia, Brazil.
Talanta. 2018 Jul 1;184:87-92. doi: 10.1016/j.talanta.2018.02.089. Epub 2018 Feb 26.
This work proposes an on-line preconcentration system using ion-imprinted polymer (IIP) for determination of bismuth in seawater employing atomic fluorescence spectrometry (AFS). The polymer was synthesized using 2- (5-bromo-2-pyridylazo) -5-diethylaminophenol (Br-PADAP) for complex formation, ethylene glycol dimethacrylate (EGDMA), cross-linking reagent and methacrylic acid (AMA) reagents, used as the functional monomer, 2,2-azobisisobutyronitrile was used as the radical initiator. The polymer was characterized employing the Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The determination of bismuth was performed employing hydride generation atomic fluorescence spectrometry (HG AFS) and the experimental conditions were optimized using a Box Behnken design involving the factors sample pH, eluent concentration and sodium tetrahydroborate concentration. So, using the optimized conditions the system allows the determination of bismuth with limits of detection and quantification of 26 and 88 ng L, a preconcentration factor of 19.8. All these parameters were determined using a sample volume of 25 mL. The precision expressed as relative standard deviation (RSD%) was 3.7% for a bismuth(III) solution of concentration 0.25 µg L. The system proposed was applied for the determination of bismuth in four seawater samples collected in Salvador City, Bahia State, Brazil. The concentrations obtained varied from 0.38 to 0.45 μg L. The accuracy was evaluated by addition/recovery test, and the recoveries found varied from 92% to 101%.
本工作提出了一种在线预浓缩系统，使用离子印迹聚合物（IIP）结合原子荧光光谱法（AFS）测定海水中的铋。聚合物的合成采用 2-（5-溴-2-吡啶偶氮）-5-二乙氨基苯酚（Br-PADAP）作为络合剂，乙二醇二甲基丙烯酸酯（EGDMA）、交联试剂和甲基丙烯酸（AMA）试剂作为功能单体，2,2-偶氮二异丁腈作为自由基引发剂。聚合物的结构特征采用傅里叶变换红外光谱（FTIR）和扫描电子显微镜（SEM）进行了表征。采用氢化物发生原子荧光光谱法（HG AFS）测定铋，并采用 Box-Behnken 设计对实验条件进行了优化，包括样品 pH、洗脱液浓度和硼氢化钠浓度等因素。在优化条件下，该系统允许在 25 mL 样品体积下，以检测限和定量限分别为 26 和 88 ng L、预浓缩因子为 19.8 的条件下测定铋。用浓度为 0.25 µg L 的铋（III）溶液测定时，相对标准偏差（RSD%）为 3.7%。该系统应用于测定巴西巴伊亚州萨尔瓦多市采集的四个海水样本中的铋，得到的浓度范围为 0.38 至 0.45 µg L。通过添加/回收试验评估了准确性，回收率在 92%至 101%之间。
