High quality surface water is critical for maintaining healthy ecosystems and ensuring safe drinking water, yet is often compromised by point and non-point contamination sources. Failed septic systems, an example of non-point source pollution, may generate pools of untreated or minimally treated wastewater that can runoff into nearby streams. There are currently no means of quickly determining the impact of this pollution on surface water. Representative emerging contaminants (caffeine and triclosan) were targeted as indicators from failed septic systems and chlorination disinfection byproducts (haloacetic acids) for the effluent from conventional municipal wastewater treatment plants. Methods for the analysis of these compounds in various matrices were developed and applied to both effluent types and surrounding surface waters. Typical caffeine and triclosan concentrations in conventional municipal wastewater treatment plant effluents were 0.23μg/L and 0.3μg/L, respectively, as compared to 22μg/L and 7μg/L from septic tank effluents. Excitation-emission fluorescence spectrophotometry was also investigated as a tool for characterizing pollution from wastewater sources.