Preparation and characterization of magnetic nanoparticles for the on-line determination of gold, palladium, and platinum in mine samples based on flow injection micro-column preconcentration coupled with graphite furnace atomic absorption spectrometry

• Magnetic nanoparticles functionalized with 4′-aminobenzo-15-crown-5-ether were synthesized.
• Experimental conditions were optimized for preconcentration of Au, Pd, Pt in an on-line system.
• The FI-column-GFAAS method was successfully applied to determine Au, Pd, and Pt in mine samples.

A simple and highly selective procedure for on-line determination of trace levels of Au, Pd, and Pt in mine samples has been developed using flow injection-column adsorption preconcentration coupled with graphite furnace atomic absorption spectrophotometry (FI-column-GFAAS). The precious metals were adsorbed on the as-synthesized magnetic nanoparticles functionalized with 4′-aminobenzo-15-crown-5-ether packed into a micro-column and then eluted with 2% thiourea+0.1 mol L−1 HCl solution prior to the determination by GFAAS. The properties of the magnetic adsorbents were investigated by scanning electron microscope (SEM), X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). Various experimental parameters affecting the preconcentration of Au, Pd, and Pt were investigated and optimized. Under the optimal experimental conditions, the detection limits of the developed technique were 0.16 ng mL−1 for Au, 0.28 ng mL−1 for Pd, and 1.01 ng mL−1 for Pt, with enrichment factors of 24.3, 13.9, and 17.8, respectively. Precisions, evaluated as repeatability of results, were 1.1%, 3.9%, and 4.4% respectively for Au, Pd, and Pt. The developed method was validated by the analysis of Au, Pd, and Pt in certified reference materials and mine samples with satisfactory results.