A study of the peculiarities of the change in the concentration of toluene in the atmospheric air of the city, where the sources of the substance are both vehicles and an industrial enterprise for the production of synthetic rubber, has been carried out. The paper analyzes the behavior of methylbenzene in different periods: with small and large volumes of industrial emissions. The sources of the substance intake are described. A diagram of the change in the emission volumes of the toluene source enterprise has been built. The periods, characterized by different industrial load on the hygienic state of the air in the city, have been determined. Statistical characteristics of data arrays of methylbenzene concentration for the periods of 2010–2012 and 2015–2017 were calculated. Wind directions are obtained showing the priority influence of the pollution source. The nature of the influence of meteorological parameters on the toluene content in the air of the residential part of the city was revealed at various volumes of the petrochemical enterprise’s emission. The study revealed a change in the influence of temperature and wind speed on the toluene content in the atmospheric air of the city under various anthropogenic load.