Universidade Federal do Recôncavo da Bahia, Centro de Ciências Exatas e Tecnológicas, Campus Universitário de Cruz das Almas, CEP 44380-000, Cruz das Almas, Bahia, Brazil.
Talanta. 2012 Jan 30;89:276-9. doi: 10.1016/j.talanta.2011.12.027. Epub 2011 Dec 19.
In the present study, a minicolumn of sisal fiber loaded with alizarin fluorine blue is proposed as a preconcentration system for copper determination in tobacco leaf samples by flame atomic absorption spectrometry. During the optimization procedure, a two level full factorial design (2(4)) was used at the preliminary evaluation of four factors, involving the following variables: sampling flow rate, elution flow rate, buffer concentration and pH. Regarding the studied levels, this design has shown that buffer concentration and pH were significant factors. The experimental conditions established in the optimization step were: pH=4.75, buffer concentration of 0.005 mol L(-1) for elution with HCl 1.0 mol L(-1) this system allows the determination of copper content with a detection limit (LD) of 0.018 μg L(-1) and a quantification limit (LQ) of 0.061 μg L(-1) precision expressed as relative standard deviation (R.S.D.) of 4.65 and 5.07%, utilizing concentration of 10 and 2.0 μg L(-1), respectively, and a preconcentration factor of 75, for a sample volume of 50.0 mL. Accuracy was confirmed by copper determination in the standard reference material, NIST SRM 1570 a trace element units in Spinach Leaves and by spike tests with recovery levels ranging from 93 to 100%; the procedure was applied for copper determination in tobacco leaf samples collected in Cruz das Almas City, Bahia, Brazil. The achieved concentrations of the three samples analyzed varied from 0.15 to 0.52 μg g(-1).
在本研究中,提出了一种用茜素氟蓝负载的剑麻纤维作为预浓缩系统,通过火焰原子吸收光谱法测定烟叶样品中的铜。在优化过程中,采用二水平完全析因设计(2(4))对四个因素进行初步评估,涉及以下变量:采样流速、洗脱流速、缓冲液浓度和 pH 值。就所研究的水平而言,该设计表明缓冲液浓度和 pH 值是重要因素。在优化步骤中确定的实验条件为:pH=4.75,洗脱时缓冲液浓度为 0.005 mol L(-1) HCl 1.0 mol L(-1)。该体系允许在铜含量检测限(LD)为 0.018 μg L(-1),定量限(LQ)为 0.061 μg L(-1)的条件下进行测定,精密度以相对标准偏差(R.S.D.)表示,分别为 4.65%和 5.07%,利用浓度为 10 和 2.0 μg L(-1),样品体积为 50.0 mL。通过在标准参考物质 NIST SRM 1570 中测定铜,该物质是菠菜叶片中的微量元素单位,以及通过加标回收试验,证明了该方法的准确性,回收率范围为 93-100%;该程序用于测定巴西巴伊亚州克鲁兹达斯阿尔马斯市采集的烟叶样品中的铜。三个分析样品的浓度变化范围为 0.15-0.52 μg g(-1)。