Spike/Leach Procedure to Prepare Soil Samples for Trace Metal Ecotoxicity Testing: Method Development Using Copper

Soil trace metal ecotoxicity testing requires a set of soil samples with increasing metal concentrations that are otherwise chemically similar. Leaching samples amended with soluble metal salts has been proposed as a means to reduce chemical artefacts of the spiking procedure (i.e., salt effect), thereby improving their environmental relevance. Demonstrating with copper (Cu), we proposed a spike/leach procedure whereby metal solutions were added to test soils over 5 days and subsequently leached with dilute nutrient solutions until the electrical conductivity in leachates stabilized. During the 5 days of Cu additions, pH in leachates from Cu-spiked samples decreased by up to 0.90 pH units and showed up to 30- and 25-fold increases in calcium (Ca) and magnesium (Mg) concentrations, indicative of the salt effect. Leaching removed the excess acidity and dissolved cations and minimized the differences in leachate pH, Ca, Mg, aluminum (Al), iron (Fe), manganese (Mn), and dissolved organic carbon (DOC) concentrations between control and Cu-spiked samples. Leaching also reduced dissolved Cu concentrations in spiked samples by up to an order of magnitude, resulting in more environmentally relevant concentrations than were achieved prior to leaching.