An expanded graphite-epoxy composite electrode (EG-Epoxy) was employed for the simultaneous determination of 4-chlorophenol (4-CP) and oxalic acid (OA) by using cyclic voltammetry (CV), chronoamperometry (CA), and differential pulse voltammetry (DPV). The results indicated that OA could be determined in the presence of the same concentrations of 4-CP within the concentration range of 0.1 mM to 0.5 mM with a relative standard deviation (RSD) smaller than 5%. Electrode fouling occurred during CA for 4-CP concentrations larger than 0.5 mM. The DPV method was used for the simultaneous determination of 4-CP and OA before and after electrochemical oxidation by chronopotentiometry under galvanostatic conditions (j ¼ 0.04 mA cm À2 , t ¼ 2 h) of a tap water sample spiked with 0.19 mM 4-CP and 0.1 M Na 2 SO 4 .