Ionic liquid-modified Fe₃O₄ nanoparticle combined with central composite design for rapid preconcentration and determination of palladium ions

Abstract

In this work, magnetic Fe₃O₄ nanoparticles (NPs) were synthesized by ultrasonic chemical co-precipitation method. Then hydrophobic ionic liquid (IL), as a green coating agent, was deposited on the surface of synthesized NPs in order to improve their extraction capability toward Pd(II) ions as diethyldithiocarbamate (DDTC) complex. Scanning electron microscopy, thermogravimetric analysis, X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and Fourier transformed infrared (FTIR) techniques were used for characterization of the adsorbent. The adsorption rate was fast and the equilibrium time was achieved within 4 min due to the strong interaction of Pd–DDTC complex with the IL and the absence of internal diffusion resistance. The separation of the adsorbent from aqueous bulk was achieved after about 2 min by a magnet, so no centrifugation or filtration was required. The effective parameters such as pH, concentration of ligand, amount of adsorbent, and the extraction time were inspected by using a central composite design in order to identify the most important parameters and their interactions. Under optimum conditions, the detection limit was 0.82 ng mL⁻¹ and the relative standard deviation (n = 10) was 2.8% for 100 ng mL⁻¹ of Pd(II). The proposed method was applied for the preconcentration of Pd(II) from road dust, liver, and water samples, and it was found that the amounts of palladium ions in dust and liver samples were 104 and 8.7 ng mL⁻¹, respectively.

Keywords:

• Central composite design
• Fe₃O₄ nanoparticles
• Ionic liquid
• Palladium

Acknowledgment

The support of this investigation by The Research Council of University of Tehran through Grant is gratefully acknowledged.