Yebra M C, Salgado J, Puig L, Moreno-Cid A
Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, 15782-Santiago de Compostela, Spain.
Anal Bioanal Chem. 2002 Oct;374(3):530-4. doi: 10.1007/s00216-002-1495-4. Epub 2002 Sep 6.
A flow injection analysis-flame atomic absorption spectrometric method for the determination of cadmium in seawater was developed with the aim of yielding a sensitive assay with a low detection limit. The method employs a field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 4-(2-pyridylazo) resorcinol. A Plackett-Burman 2(7)x3/32 design for seven factors (sample pH, sample flow rate, eluent volume, eluent concentration, eluent flow rate, ethanol percentage in the eluent and minicolumn diameter) was carried out in order to find the significant variables affecting the field continuous preconcentration system (FCPS) and the flow injection elution manifold for cadmium determination in seawater samples by flame atomic absorption spectrometry. Cadmium can be preconcentrated with an enrichment factor of 1053 for a sample volume of 200 mL and a preconcentration time of 57 min. In these experimental conditions, the method provides a linear relationship between absorbance and cadmium concentration in the range from 22-1900 ng L(-1), with a detection limit (3SD) of 6 ng L(-1). The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 8.9-0.8% in cadmium solutions of 50-700 ng L(-1). Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified value. This procedure was applied to the determination of cadmium in seawater from Galicia (Spain).
为了建立一种检测限低且灵敏的分析方法,开发了一种流动注射分析-火焰原子吸收光谱法用于测定海水中的镉。该方法采用了一种场流预富集技术,涉及一个装有浸渍有络合剂4-(2-吡啶偶氮)间苯二酚的Amberlite XAD-4的微型柱。为了找出影响场连续预富集系统(FCPS)和流动注射洗脱流路以通过火焰原子吸收光谱法测定海水样品中镉的显著变量,对七个因素(样品pH值、样品流速、洗脱液体积、洗脱液浓度、洗脱液流速、洗脱液中乙醇百分比和微型柱直径)进行了Plackett-Burman 2(7)x3/32设计。对于200 mL的样品体积和57分钟的预富集时间,镉的预富集因子可达1053。在这些实验条件下,该方法在22-1900 ng L(-1)范围内吸光度与镉浓度呈线性关系,检测限(3SD)为6 ng L(-1)。在50-700 ng L(-1)的镉溶液中,十一次独立测定的精密度(以相对标准偏差表示)为8.9-0.8%。对有证标准物质(SLEW-3和NASS-5)的分析结果与认定值吻合良好。该方法应用于西班牙加利西亚海水样品中镉的测定。