This study compared 3 commonly used quenching agents for dechlorinating samples prior to disinfection byproduct (DBP) analysis under typical drinking water sampling conditions for a representative suite of chlorination byproducts. Ascorbic acid and sodium sulfite quenched the residual free chlorine to below detection within 5 seconds. Ammonium chloride did not quench the chlorine to below detection with up to a 70% molar excess, which agrees with published ammonium chloride-chlorine chemistry. With respect to the DBPs, ascorbic acid worked well for the trihalomethanes and haloacetic acids, except for dibromoiodomethane, which exhibited 2.6–28% error when using ascorbic acid compared to non-quenched control samples. Sodium sulfite also worked well for the trihalomethanes (and performed similarly to ascorbic acid for dibromoiodomethane) and was the best performing quenching agent for MX and the inorganic DBPs, but contributed to the decay of several emerging DBPs, including several halonitromethanes and haloacetamides. Ammonium chloride led to considerable errors for many DBPs, including 27–31% errors in chloroform concentrations after 24 hours of storage. This work shows that ascorbic acid is suitable for many of the organic DBPs analyzed by gas chromatography-electron capture detection and that sodium sulfite may be used for simultaneous chlorite, chlorate, and bromate analysis.