A sensor was developed for the first time based on polydopamine nanospheres doped with I2, I−, and IO3 − species (PDA-Iodine), to determine the concentration of p-aminophenol (p-AP), phenol (Ph), and p-nitrophenol (p-NP) simultaneously. These polymeric nanospheres were successfully characterized using a variety of techniques including field emission scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared, Raman spectroscopy, and X-ray diffraction analysis. A carbon paste electrode was modified with the PDA-Iodine (CPE/PDA-Iodine). Because of the electrocatalytic activity of DA/DQ, I2 and I− species (in the structure of PDA-Iodine), CPE/PDA-Iodine shows enhancement in the electrooxidation peak currents as well as slight negative shift in peak potentials of p-AP, Ph, and p-NP compared with a bare carbon paste electrode. Under optimal experimental conditions, the linear calibration plots are linear in the ranges 0.5–120 μM for p-AP, 0.7–120 μM for Ph, and 1.0–100 μM for p-NP with limits of detection of 30, 40, and 80 nM for p-AP, Ph, and p-NP, respectively (S/N = 3). To prove the performance of the method, the repeatability of the signals of CPE/PDA-Iodine was evaluated and the RSD values obtained were 2.9%, 3.2%, and 3.1% for p-AP (45 μM), Ph (40 μM), and p-NP (40 μM), respectively. The CPE/PDA-Iodine is a promising new sensor for sensing p-AP, Ph, and p-NP simultaneously in tap and river water sample and the values of recoveries for spiked samples were in the range 94.0–104.4%.

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