Vernadsky Institute of Geochemistry and Analytical Chemistry, Russian Academy of Sciences, Kosygin Street 19, 119991 Moscow, Russia.
Talanta. 2012 Jan 15;88:369-74. doi: 10.1016/j.talanta.2011.11.002. Epub 2011 Nov 9.
Dynamic fractionation is considered to be an attractive alternative to conventional batch sequential extraction procedures for partitioning of trace metals and metalloids in environmental solid samples. This paper reports the first results on the continuous-flow dynamic fractionation of selenium using two different extraction systems, a microcolumn (MC) packed with the solid sample and a rotating coiled column (RCC) in which the particulate matter is retained under the action of centrifugal forces. The eluents (leachants) were applied in correspondence with a four-step sequential extraction scheme for selenium addressing "soluble", "adsorbed", "organically bound", and "elemental" Se fractions extractable by distilled water, phosphate buffer, tetramethylammonium hydroxide, and sodium sulphite solutions, respectively. Selenium was determined in the effluent by using an inductively coupled plasma atomic emission spectrometer. Contaminated creek sediment and dumped waste (soil) samples from the abandoned mining area were used to evaluate resemblances and discrepancies of two continuous-flow methods for Se fractionation. In general, similar trends were found for Se distribution between extractable and residual fractions. However, for the dumped waste sample which is rich in organic matter, the extraction in RCC provided more effective recovery of environmentally relevant Se forms (the first three leachable fractions). The most evident deviation was observed for "adsorbed" Se (recoveries by RCC and MC are 43 and 7 mg kg(-1), respectively). The data obtained were correlated with peculiarities of samples under investigation and operational principles of RCC and MC.
动态分级被认为是一种有吸引力的替代传统批处理顺序提取程序,用于环境固体样品中痕量金属和类金属的分配。本文报告了使用两种不同的提取系统,即填充有固体样品的微柱 (MC) 和在离心力作用下保留颗粒物质的旋转盘管柱 (RCC),对硒进行连续流动动态分级的初步结果。洗脱液(浸提剂)应用于针对硒的四步顺序提取方案,分别提取“可溶”、“吸附”、“有机结合”和“元素”硒分数,分别使用蒸馏水、磷酸盐缓冲液、四甲基氢氧化铵和亚硫酸钠溶液提取。通过电感耦合等离子体原子发射光谱仪在流出物中测定硒。受污染的小溪沉积物和废弃矿区的倾倒废物(土壤)样品用于评估两种连续流动硒分级方法的相似性和差异。一般来说,可提取和残留部分之间的硒分布趋势相似。然而,对于富含有机物的倾倒废物样品,RCC 中的提取更有效地回收了与环境相关的硒形态(前三个可浸提分数)。对于“吸附”硒(RCC 和 MC 的回收率分别为 43 和 7 mg kg(-1)),观察到最明显的偏差。所得数据与所研究样品的特点以及 RCC 和 MC 的操作原理相关联。