One-pot/one-step synthesis of Bi2O3/ZnO/Pd nanocomposite for preconcentration and determination of some heavy metal ions in different samples

Abstract

ABSTRACT In this contribution, a new green eco-friendly synthesised nanocomposite (Bi2O3/ZnO/Pd) was fabricated by one-pot/one-step method, using ultrasonic waves. The nanocomposite was used for pre-concentration of some heavy metals, i.e. cadmium (II), lead (II), and copper (II), exploiting ultrasound-assisted dispersive micro solid phase extraction (UA-D-μ-SPE) method, before their determination by flame atomic absorption spectroscopy (FAAS). The adsorbent synthesis was confirmed by XRD, SEM, BET, TEM, EDS, and TGA analyses. The central composite design (CCD) method was employed to optimise various parameters affecting the extraction of heavy metals. The effective parameters in the adsorption process, viz. the amount of adsorbent (16 mg), pH of the sample solution (6.2), and adsorption time (4 min), were optimised. The type and the concentration of eluting agent (HCl solution) was investigated as one parameter at a time. Impressive parameters in the desorption stage such as the volume and concentration of eluting solution (400 μL of 0.8 mol L−1 HCl) and desorption time (2.5 min) were optimised. In the best extraction conditions for cadmium (II), lead (II), and copper (II), the limits of detection (LODs) were 0.75, 2.1, and 0.90 ng mL−1; the limits of quantification (LOQs) were 2.5, 7.0, and 3.0 ng mL−1; the linear dynamic ranges (LDRs) were 2.5–100, 7.0–600, and 3.0–250 ng mL−1; preconcentration factors (PF) were 24.10, 25.20, and 25.39; and the relative standard deviations (RSDs%) were 3.7, 4.1, and 3.8 (n = 5), respectively. Additionally, the adsorbent had the ability to extract metals up to 8 times without a significant decrease in the extraction percentages. The adsorbent was successfully used in the determination of cadmium (II), lead (II), and copper (II) ions in different food, biological, cosmetic, and water samples.