In the present report, TiO2 NPs were synthesized using environmental benign and cost-effective way by utilizing green route synthesis method. Structural characterization of Ficus Benjamina leaf extract-mediated TiO2 NPs [FEBLE: TiO2 NPs] revealed that as-synthesized NPs exhibit polymorphs of anatase ( I 4 2 a m d ) and rutile ( P 4 / 2 m n m ) crystal phases as confirmed through Rietveld refinement studies. FTIR spectra of biogenic TiO2 NPs shows presence of phenolic content as broadband appeared at 3400 cm−1, which confirms that Ficus Benjamina leaf extract acts as capping, reducing, and stabilizing agent. Microstructural studies depict homogeneous distribution of TiO2 grains with average grain of 22.05 ± 0.82 nm as evaluated using statistical analysis. Biosynthesized TiO2 NPs are used to detect heavy metals in industrial waste water collected from various regions of Punjab, India. The efficacy of TiO2 NPs in heavy metal detection in waste water collected from textile, steel, and chemical industries at different concentrations of 0.1 g/L, 0.5 g/L, and 1 g/L with 90–120 min of the exposure time was investigated. At a concentration of 1 g/L of TiO2 NPs, maximum efficiency for metal detection is observed in order: Pb, Zn, Cd, and Cr at 90 min of the exposure time. [ABSTRACT FROM AUTHOR]