Faculty of Chemistry, Department of Analytical Chemistry and Instrumental Analysis, Maria Curie-Sklodowska University, Maria Curie-Sklodowska Sq 3, 20-031 Lublin, Poland.
Talanta. 2010 Sep 15;82(4):1325-31. doi: 10.1016/j.talanta.2010.06.049. Epub 2010 Jul 4.
Slurry sampling atomic absorption spectrometry with electrothermal atomization was used to the determination of cadmium (Cd) and lead (Pb) in soils and sediments using permanent modifiers. Comparison of action of mixed permanent modifiers niobium (Nb)/iridium (Ir) and tungsten (W)/iridium (Ir) were studied in detail. The effect of amount of Ir, W and Nb on analytical signals of Cd and Pb was examined. The optimal amounts of modifiers for Cd and Pb determination were stated. Niobium carbide formation on graphite surface was studied for different pyrolysis temperatures. Finally for Cd determination in sediments and soils 200 microg of Nb mixed with 5 microg of Ir was used as permanent modifiers and 15 microg of Nb mixed with 200 microg of Ir for Pb determination. Suspensions were prepared in 5% HNO(3). The analytical procedure was optimized carefully basing on data from pyrolysis and atomization curves studies. Ammonium dihydrogen phosphate was used additionally as matrix modifier during Cd determination in samples in order to prevent interferences coming from matrix components. The analysis of CRMs confirmed the reliability of the proposed approach. The precision and accuracy of Cd and Pb determination by the described method for soils and sediments were acceptable.
采用浆状进样原子吸收光谱法,用电热原子化法,使用永久性修饰剂测定土壤和沉积物中的镉(Cd)和铅(Pb)。详细研究了混合永久性修饰剂铌(Nb)/铱(Ir)和钨(W)/铱(Ir)的作用。考察了 Ir、W 和 Nb 的量对 Cd 和 Pb 分析信号的影响。确定了用于 Cd 和 Pb 测定的最佳修饰剂用量。研究了不同热解温度下石墨表面碳化铌的形成情况。最后,对于沉积物和土壤中 Cd 的测定,使用 200μg Nb 与 5μg Ir 混合作为永久性修饰剂,而对于 Pb 的测定,则使用 15μg Nb 与 200μg Ir 混合。悬浮液在 5% HNO3 中制备。根据热解和原子化曲线研究的数据,仔细优化了分析程序。为了防止基质成分引起的干扰,在测定样品中的 Cd 时,还额外使用了磷酸二氢铵作为基质修饰剂。对 CRMs 的分析证实了所提出方法的可靠性。所描述方法用于土壤和沉积物中 Cd 和 Pb 的测定具有可接受的精密度和准确度。