In this study, gold nanoparticles (AuNPs) were electrodeposited on samples of a carbon-paste electrode (CPE) with different thicknesses. The prepared AuNPs were characterized using different analysis techniques, such as FTIR, UV‒Vis, SEM, EDX, TEM images, and XRD analysis. The fabricated modified electrode AuNPs/CPE was used for the sensitive detection of Congo red (CR) dye. Electrochemical sensing was conducted using square-wave voltammetry (SWV) in a 0.1 M acetate buffer solution at pH 6.5. The proposed sensor exhibited high efficiency for the electrochemical determination of CR dye with high selectivity and sensitivity and a low detection limit of 0.07 μM in the concentration range of 1–30 μM and 0.7 μM in the concentration range of 50–200 μM. The practical application of the AuNPs/CPE was verified by detecting CR dye in various real samples involving jelly, candy, wastewater, and tap water. The calculated recoveries (88–106%) were within the acceptable range.
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