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In this study, a facile protocol was used to convert non-valuable orange peels (OP) waste into a new sensing iron oxide orange-peel nanomaterial (FeOP). The presence of iron oxide nanoparticles in the modified OP was confirmed by physicochemical characterisations including Fourier-transform infrared spectroscopy, X-ray diffractometry, thermogravimetry, and scanning electron microscopy-energy dispersive X-ray. FeOP was used to modify a carbon paste electrode (CPE/FeOP) which displayed a significant increase in specific capacitance of 2939 F.g−1, two folds higher than that obtained with CPE at 10 m.s−1 in NaCl. The electroanalysis of Congo red (CR) in aqueous solutions using CPE/FeOP displayed detection limits of 2.8 × 10−7 mol.L−1 and 8.2 × 10−7 mol.L−1 respectively in deionised and spring waters, in the linear range of 5 to 55 µM. CPE/FeOP electrochemical sensor is therefore suitable for the determination of Congo red in wastewater.