In this study, a small bench‐scale plug‐flow reactor was designed and characterized to demonstrate the feasibility of using UV/LEDs as a UV source in flow‐through advanced oxidation processes. The plug‐flow reactor was characterized by investigating the effects of residence time, H2O2/methylene blue molar ratio, and initial methylene blue concentration on methylene blue decolorization in water. Methylene blue was selected as a witness dye, because it does not degrade with H2O2 or with UV alone, and it has reduced absorption in the visible spectrum when reacted with OH radicals. UV/LEDs have been employed successfully in AOPs for water treatment in research‐scale systems, as demonstrated in this study. However, they currently have low optical output, which limits their applicability for water treatment to small point‐of‐use systems. © 2017 American Institute of Chemical Engineers Environ Prog, 36: 857–863, 2017