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One hundred and seventeen street sweeping samples were collected and analyzed for per- and polyfluoroalkyl substances (PFAS). Fifty-six samples were collected in one city (Gainesville, Florida) allowing for an in-depth city-wide characterization. Street sweepings from five other urban areas, (Orlando, n = 15; Key West, n = 15; Pensacola, n = 12; Tampa, n = 13; and Daytona Beach, n = 6) were analyzed to provide a city-to-city comparison of PFAS. Within our analytical workflow, 37 PFAS were quantified across all samples, while the maximum number of PFAS quantified at one site was 26. Of those PFAS quantified in Gainesville, 60% were perfluoroalkyl acids (PFAAs) and 33% were precursors to PFAA. Among the PFAAs, short-chain perfluoroalkyl carboxylic acids (PFCAs) were the dominant class representing 26% of the total PFAS by concentration. In the comparison across different urban cities, the dominant compound by concentration and frequency of detection varied; however, perfluorooctanoic acid (PFOA) and linear perfluorooctanesulfonic acid (PFOS lin ) were the two PFAS that were detected the most frequently. This study documents the first-time detection of hexadecafluorosebacic acid and perfluoro-3,6,9-trioxaundecane-1,11-dioic acid within environmental samples.