Felipe-Sotelo M, Carlosena A, Fernández E, López-Mahía P, Muniategui S, Prada D
Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira s/n E-15071, A Coruña, Spain.
Talanta. 2004 Jun 17;63(3):735-42. doi: 10.1016/j.talanta.2003.12.029.
Slurry sampling is compared to microwave-assisted acid digestion for cobalt determination in soil/sediment samples by electrothermal atomic absorption spectrometry (ETAAS). Furnace temperature programs and appropriate amounts of three chemical modifiers were optimised in order to get the highest signals and good separations between the atomic and background signals. Using nitric acid (0.5% (v/v)) as liquid medium, no chemical modifier was needed. The detection limit, based on integrated absorbance, was 0.04mugg(-1) for digests and slurries. Within-batch precision and analytical recoveries were satisfactory for both procedures. Accuracy was tested by analysing a reference soil and a sediment from IRMM. The methods were further compared employing a set of roadside soils and estuarine sediments. As no significant differences (95% confidence) were found, practical analytical properties were suggested in order to select one of them.
通过电热原子吸收光谱法（ETAAS），比较了悬浮液进样和微波辅助酸消解用于测定土壤/沉积物样品中的钴。优化了炉温程序和三种化学改进剂的合适用量，以获得最高信号以及原子信号与背景信号之间的良好分离。使用硝酸（0.5%（v/v））作为液体介质时，无需化学改进剂。基于积分吸光度，消解液和悬浮液的检测限均为0.04μg g⁻¹。两种方法的批内精密度和分析回收率均令人满意。通过分析IRMM的一种参考土壤和一种沉积物来测试准确度。使用一组路边土壤和河口沉积物进一步比较了这些方法。由于未发现显著差异（95%置信度），因此提出了实际分析特性以便从中选择一种方法。
