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The increasing prevalence of hazardous chemical incidents in the United States necessitates the implementation of analytically robust, rapid, and reliable screening techniques for toxicant mixture analysis to understand short- and long-term health impacts of environmental exposures. A recent chemical disaster in East Palestine, Ohio has underscored the importance of thorough contamination assessment. On February 03, 2023, a Norfolk Southern train derailment prompted a chemical spill and fires. An open burn involving over 100,000 gal of vinyl chloride was conducted three days later. Hazardous compounds were released into air, water, and soil. To provide time-sensitive exposure data for emergency response, this study outlines a novel methodology for rapid characterization of chemical contamination of environmental media to support disaster response efforts. A controlled static headspace sampling system, in conjunction with a high-resolution proton transfer reaction time-of-flight mass spectrometer (PTR-TOF-MS), was developed to characterize volatile organic compounds (VOCs) in surface water samples collected near the East Palestine train derailment site. Spatial variations were observed in the chemical composition of surface water samples collected at different locations. Hydrocarbons were found to be the most abundant chemical group of all surface water samples, contributing 50 % to 97 % to the total headspace VOC mass. Compounds commonly detected in surface water samples, including benzene, styrene, xylene, and methyl tert-butyl ether (MTBE) were also observed in most surface water samples, with aqueous concentrations typically at ng/L levels. This study demonstrated the potential of the proposed methodology to be applied for rapid field screening of volatile chemicals in water samples in order to enable fast emergency response to chemical disasters and environmental hazards.