The electrochemical oxidation of cibacron red FN-R (CB) has been studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) at a glassy carbon electrode (GCE) in phosphate buffer solutions of pH (2.54- 11.79) used as supporting electrolyte. The voltammetric behaviour showed that the electro-oxidation process gave rise to a single peak at 0.692 V vs. Ag-AgCl using DPV in phosphate buffer solution at (pH 3.34). The oxidation process was shown to be irreversible and adsorption-controlled. An analyticalmethod was developed for the determination of cibacron red FNR in phosphate buffer solution at (pH 3.34) as supporting electrolyte. The anodic peak current varied linearlywith cibacron red FN-R concentration in the range 2.0ï´10-6mol/l to 1.0ï´10-5mol/l of cibacron red FN-Rwith a limit of detection (LOD) of 4.49ï´10-7 mol/l and limit of quantification (LOQ) of 1.49ï´10-6 mol/l. Validation parameters, such as accuracy, precision and recovery were evaluated. The proposed method was successfully applied to the determination of cibacron red FN-R in synthetic industrial effluents and the analytical results compared well with those obtained by the spectrophotometric method.