The feasibility of using novel electromagnetic wave sensors for real-time monitoring of metal pollution in water was assessed. Five solutions with different concentrations of lead (0, 1, 10, 50, 100 mg/L) were measured using several sensing methods: UV-Vis spectroscopy, low frequency capacitance and resistance measurements, and two sensing systems based on microwave technology. With this last approach, two sensing devices were used: a resonant cavity and a planar sensor with gold interdigitated electrode design printed on a PTFE substrate with a protective PCB lacquer coating. Results confirmed the ability of these systems to quantify the lead concentration as changes in spectrum signal at specific frequencies of the electromagnetic spectrum. Spectra were unique, with clearly observed shifts in the resonant frequencies of the sensors when placed in direct contact with different lead solutions, demonstrating the possibility of continuous monitoring with great sensitivity, selectivity, and high spatial and temporal resolution. Consequently, determination of trace and toxic metals using microwave spectroscopy is a promising alternative to traditional grab-sampling and laboratory based analyses. On-line and continuous monitoring of real-time metal concentrations offers the potential for a more effective emergency response and the platform for better scientific understanding and remediation of contaminated mine drainage.