Natural and anthropogenic disasters are associated with air quality concerns due to the potential redistribution of pollutants in the environment. Our objective was to conduct a spatiotemporal analysis of air concentrations of benzene, toluene, ethylbenzne, and xylene (BTEX) and criteria air pollutants in North Carolina during and after Hurricane Florence. Three sampling campaigns were carried out immediately after the storm (September 2018) and at four-month intervals. BTEX were measured along major roads. Concurrent criteria air pollutant concentrations were predicted from modeling. Correlation between air pollutants and possible point sources was conducted using spatial regression. Exceedances of ambient air criteria were observed for benzene (in all sampling periods) and PM2.5 (mostly immediately after Florence). For both, there was an association between higher concentrations and fueling stations, particularly immediately after Florence. For other pollutants, concentrations were generally below levels of regulatory concern. Through characterization of air quality under both disaster and “normal” conditions, this study demonstrates spatial and temporal variation in air pollutants. We found that only benzene and PM2.5 were present at levels of potential concern, and there were localized increases immediately after the hurricane. These substances warrant particular attention in future disaster response research (DR2) investigations.