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We explored a novel technique to deploy solid-phase microextraction (SPME) fibers to nondestructively measure the explosive compound 2,4,6-trinitrotoluene (TNT) and its nitroaromatic (NA) degradation products in laboratory sediment toxicity tests and field sediments in situ. SPME fibers within steel mesh envelopes were exposed statically via direct burial within sediment. Six fiber types (polymer coatings) were tested. Polyacrylate (PA) SPME fiber was sufficiently durable for this application, yielded the lowest detection limits, and exhibited a linear uptake relationship across toxicologically relevant sediment NA concentrations (100−2000 nmol/g dw (20−500 μg/g dw)). Temperature greatly influenced SPME absorption kinetics. Via evaluation of absorption at different temperatures, recommended sampling times needed to achieve steady-state equilibrium were 48 h for room temperatures (23−25 °C) and up to 7 d for …