This study presents the design and application of an electrochemical sensor for selective detection of lead ions (Pb2+) based on ionophore-modified raspberry-like Fe3O4–Au nanostructures. The material was engineered with a magnetic Fe3O4 core, coated with polyethyleneimine (PEI) to facilitate nucleation, and subsequently decorated with Au nanoparticles, providing a raspberry-like (Fe3O4@PEI@AuNPs) nanostructure with high surface area and excellent electrochemical conductivity. Surface functionalization with Lead Ionophore IV (ionophore thiol) introduced Pb2+-selective binding sites, whose presence and structural evolution were verified by TEM and Raman spectroscopy. The Fe3O4 core endowed strong magnetic properties, enabling facile manipulation and immobilization onto screen-printed carbon electrodes (SPCEs) via physical adsorption, while the Au nanoparticles enhanced electron transfer, supplied thiol-binding sites for stable ionophore anchoring, and increased the effective electroactive surface area. Operational conditions were systematically optimized, with acetate buffer (HAc/NaAc, pH 5.7) and chronoamperometric preconcentration (CA) at −1.0 V for 175 s identified as optimal for differential pulse voltammetry (DPV) measurements. Under these conditions, the sensor exhibited a linear response toward Pb2+ from 0.025 mM to 2.00 mM with superior sensitivity and reproducibility compared to conventional AuNP-modified SPCEs. Furthermore, the ionophore-modified Fe3O4–Au nanostructure-based sensor demonstrated outstanding selectivity for Pb2+ over competing heavy metal ions (Cd2+, Hg2+, Cr3+), owing to the specific coordination interaction of Lead Ionophore IV with target ions. These findings highlight the potential of raspberry-like Fe3O4@PEI@AuNP nanostructures as a robust and efficient electrochemical platform for the sensitive and selective detection of toxic heavy metal ions.
A facile approach was employed for the synthesis of cobalt oxide nanorods (NRs) using cobalt nitrate, sodium oxalate and ethylene glycol as precursors via a hydrothermal process. The hydrothermal conditions, such as temperature and time, were varied to optimize the morphological characteristics of the NRs. After undergoing filtration, washing, and drying, the resulting material was characterized using several techniques, including field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and transmission electron microscopy (TEM). Our findings reveal that the NRs exhibit diverse morphologies, depending on the hydrothermal conditions, with the smallest aspect ratio observed when prepared at 200 °C for 24 hours. In addition, we investigated the gas sensing capabilities of the NRs to ammonia under these conditions.