Multistep Method to Extract Moderately Soluble Copper Oxide Nanoparticles from Soil for Quantification and Characterization.

The objective of this study is to assess how method parameters impact the extraction of moderately soluble CuO nanoparticles (NPs) from a standard natural soil (LUFA 2.1) suitable for chemical analysis. The extraction procedure is comprised of three steps: (i) preconditioning the soil to increase the sodium adsorption ratio, (ii) extracting colloids/NPs from the soil matrix using sonication and a dispersing agent, and (iii) separating the dissolved and nanoparticulate CuO fractions using cloud point extraction. Method parameters of the extraction procedure, including sonication, number of extraction cycles, and dispersing agent, were adjusted to achieve the highest extraction of CuO NPs, while minimizing dissolution. The maximum recovery of CuO NPs ranged from 31% to 42% for an amended concentration range of 10-250 mg-Cu (kg soil)-1 using a preconditioning step to exchange divalent cations for monovalent ions, 0.2% carboxymethyl cellulose (CMC) 700 kg mol-1 as the dispersing agent, probe sonication for 1 min, 3 extraction cycles, and a 1:10 soil-to-liquid ratio. CuO NPs that are polyvinylpyrrolidone (PVP)-coated with a greater stability against aggregation had significantly higher extractability and dissolution. This procedure is the first to effectively extract moderately soluble NPs from soil and experimentally separate them from their dissolved fraction and can be applied to other moderately soluble metal containing natural, incidental, or engineered NPs in soil.