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In order to determine the condition of drinking water sources in Donetsk Region and assess potential threats related to water pollution from mining and industrial wastewater, it is extremely important to monitor surface waters, which should include an assessment of the condition of gydrobionts. Additionally, declining surface water quality in the region contributes to pollution in the coastal waters of the Sea of Azov. This study presents the monitoring results for the southern part of the Kalmius River basin. Analysis of water samples revealed contamination by phenol, sulfates, chlorides, anionic surfactants, iron, elevated water hardness, and significant exceedances of suspended solids and total dissolved solids. The iron concentration at the Kalmius River estuary reached 0.81 mg∙L⁻¹, exceeding the permissible limit by 2.5-fold. Sulfate and total dissolved solids concentrations attained 1673 and 160 mg∙L⁻¹, respectively. Changes in the species composition of phytoplankton were observed in response to variations in iron, manganese, and phenol concentrations in the water. Specifically, elevated iron levels led to increased abundance of the metal-sensitive species Cyclotella meneghiniana Kützing. Principal component analysis of the data revealed a relationship between increased phenol concentrations in the aquatic environment and a mean 20% reduction in phytoplankton cell photosynthetic activity, as well as the influence of manganese ions on cell abundance and photopigment content. Thus, phytoplankton cell fluorescence, alongside shifts in species composition and photosynthetic pigment content, can serve as an additional indicator of surface water pollution by iron and phenol. Full article