A facile hydrothermal process was used to prepare nanostructures of ZnO/Yb 2 O 3 in alkaline medium, which were applied for efficient chemical sensor development. The sensor fabricated with ZnO/Yb 2 O 3 nanostructures may be a promising sensitive chemical sensor for the effective detection of environmental effluents. In this study, a facile hydrothermal process was used to prepare the NSs of ZnO/Yb 2 O 3 in an alkaline medium (pH ∼ 10.5), at a low temperature. The calcined NSs were characterized by Fourier-transform infrared spectroscopy (FTIR), ultraviolet visible spectroscopy (UV/vis), field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and powder X-ray diffraction (XRD). A thin layer of NSs was coated on a glassy carbon electrode (GCE) with the help of a nafion conducting binder to be used as a sensor. This assembled sensor was implemented to the successful detection of 4-AP and exhibited good sensitivity (5.063 μA μM −1 cm −2 ) and a low detection limit (DL = 0.019 ± 0.001 nM at a signal to noise ratio of 3). The calibration plot (attained at a potential of +1.0 V) is linear ( r 2 = 0.9836) in the concentration range of 0.1 nM to 0.1 mM of 4-AP. Therefore, the chemical sensor fabricated with ZnO/Yb 2 O 3 NSs may be a promising sensitive chemical sensor in a reliable I – V method for the effective detection of hazardous and carcinogenic chemicals in environmental and healthcare sectors on broad scales.