Recent advances in nanotechnology have led to the production of materials with nanoscale dimensions (nm) and properties distinctly different from their bulk (>100 nm) counterparts. With increased use, it is inevitable that nanomaterials will accumulate in the environment and there is concern that the novel properties of nanomaterials could result in detrimental environmental and human health effects. In particular, there has been concern recently regarding the use of silver (Ag) based nanomaterials as antimicrobial agents in consumer and medical products. Current regulations dealing with the discharge of metals into the environment are based on total concentrations with no consideration for the form (e.g., ionic, nanoparticle, colloid) which can largely determine toxicity. Methods for the identification and characterization of nanoparticulates within complex matrices are lacking and the development of robust methods for this purpose are considered a high priority research area. This research focuses on the development and application of a novel method for characterizing Ag manufactured nanoparticles (MNPs) within terrestrial environments, in particular in soil pore water, with applications relevant to other metal MNPs as well. The method was then applied to understand the dynamics and behavior of Ag MNPs in soil and soil amended with sewage sludge biosolids.