Dynamic Four-step Sequential Extraction Procedure Using a Four-channel Circulating Flow System for Extracting Cd, Cu, Pb, and Zn from Solid Environmental Samples.

A method for extracting metals from solid samples was developed. The system had four flow channels (each containing a column packed with a solid sample), a single-flow peristaltic pump, and eight six-port valves. An extractant was passed into each channel for a specified period, then the valves were closed. We evaluated the system by performing a four-step sequential extraction procedure to extract heavy metals from a lake sediment sample. The four extractants were, in order of use, magnesium chloride, ammonium acetate, hydroxylamine hydrochloride, and hydrochloric acid. The concentrations of the analytes extracted agreed well with the concentrations determined using the batch method. The system was also successfully used to analyze heavy metals in a soil sample from a parking lot and fly ash from a domestic waste disposal facility. The total amount of extractant required per sample using the system was two-thirds of the amount required using the batch method.

Monitoring of the Palladium Concentration in River Water and Sediment at an Acidic Hot Spring Spa Area in Gunma Prefecture.

In an effort to elucidate the deposition pathway of Pd in river sediments, we analyzed the amount of Pd in the river water and sediments of the Yukawa and Yazawa rivers, as well as in the sediments of the Shinaki dam-lake of the Kusatsu hot-spring area, which is located northwest in Gunma Prefecture of Japan. The crystal structures and elemental compositions of the river sediment samples differed significantly before and after neutralization. This was attributed to the lime input, which also affected the Pd abundance ratio obtained by the sequential extraction procedure. Additionally, the low leachability of Pd in the sediment suggested possible difficulties in its recovery. Considering the analysis of the Pd variation in the environments, it was concluded that the Pd content in the sediment of the Shinaki dam-lake was mainly supplied by the Yukawa river water inflowing the surrounding tributary rivers and hot-spring waters before neutralization, rather than the lime input.

Dynamic leaching and fractionation of trace elements from environmental solids exploiting a novel circulating-flow platform.

A dynamic flow-through microcolumn extraction system based on extractant re-circulation is herein proposed as a novel analytical approach for simplification of bioaccessibility tests of trace elements in sediments. On-line metal leaching is undertaken in the format of all injection (AI) analysis, which is a sequel of flow injection analysis, but involving extraction under steady-state conditions. The minimum circulation times and flow rates required to determine the maximum bioaccessible pools of target metals (viz., Cu, Zn, Cd, and Pb) from lake and river sediment samples were estimated using Tessier's sequential extraction scheme and an acid single extraction test. The on-line AIA method was successfully validated by mass balance studies of CRM and real sediment samples. Tessier's test in on-line AI format demonstrated to be carried out by one third of extraction time (6h against more than 17 h by the conventional method), with better analytical precision (<9.2% against >15% by the conventional method) and significant decrease in blank readouts as compared with the manual batch counterpart.