Non-aqueous phase liquids (NAPL) are a complex group of environmental contaminants which pose a challenge to environmental managers. Nuclear magnetic resonance (NMR) spectroscopy has potential applications in this field but is currently underutilized. This thesis aims to assess and improve the ability of NMR for NAPL analysis. Specifically, a novel 1H NMR fingerprinting scheme was developed for polycyclic aromatic hydrocarbons (PAH) and was found to enhance the characterization of coal tars, while passive sampling and solid phase extraction (SPE) were explored as sample preparation techniques for dilute NAPL-contaminated water samples in conjunction with low-field benchtop NMR. Additionally, NMR was used to examine the composition of a reconstructed chlorobenzene NAPL as it underwent a series of partitioning processes including dissolution, sorption, and volatilization, to reveal the components that were most and least resistant to abiotic attenuation. These results showed promise for NMR as a tool within the context of environmental characterization and forensics of complex mixtures.