Decomposition of organic-rich bottom sediment in a tidal creek in Maryland results in production of gas bubbles in the bottom sediment during summer and fall. In areas where volatile organic contaminants discharge from ground water, through the bottom sediment, and into the creek, part of the volatile contamination diffuses into the gas bubbles and is released to the atmosphere by ebullition. Collection and analysis of gas bubbles for their volatile organic contaminant content indicate that relative concentrations of the volatile organic contaminants in the gas bubbles are substantially higher in areas where the same contaminants occur in the ground water that discharges to the streams. Analyses of the bubbles located an area of previously unknown ground-water contamination. The method developed for this study consisted of disturbing the bottom sediment to release gas bubbles, and then capturing the bubbles in a polyethylene bag at the water-column surface. The captured gas was transferred either into sealable polyethylene bags for immediate analysis with a photoionization detector or by syringe to glass tubes containing wires coated with an activated-carbon adsorbent. Relative concentrations were determined by mass spectral analysis for chloroform and trichloroethylene.