Chlorine in various forms remains the primary disinfection method for municipal water systems. Chlorine can form µg/L levels of disinfection byproducts (DBPs) in water supplies, which include haloacetic acids (HAAs). These HAAs are thought to pose potential cancer risks with high levels of exposure. As a precaution, the US EPA has defined a maximum threshold of HAA content in municipal waters. To address the need for measuring low µg/L levels of various haloacetic acids, a method was developed using ion chromatography/mass spectrometry (IC/MS), which conforms to US EPA Method 557. The benefit of using MS/MS with a triple-quadrupole mass spectrometer over using MS with a single quadrupole mass spectrometer is the ability to avoid potential interferences while achieving lower detection limits and enhanced selectivity.