ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Determination of lead and cadmium by magnetic solid-phase extraction (MSPE) using Co₃O₄@Fe₃O₄ nanoflowers and flame atomic absorption spectrometry (FAAS)

Şeyma Korkmaz, Nurdan Kurnaz Yetim, Mümin Mehmet Koç, and Cemile Özcan

Department of Chemistry, Faculty of Arts and Sciences, Kırklareli University, Kırklareli, Türkiye

E-mail: cemilebal.ozcan@klu.edu.tr

Received: 8 July 2023  Accepted: 9 March 2024

Abstract:

Heavy metal ions penetrate wastewater and clean water sources, leading to environmental pollution which adversely affecting human health. The determination and extraction of metal ions help to prevent unwanted effects on the environment and human health. Solid phase extraction method is used for the removal of heavy metal ions. Such method is rapid, reliable and affordable method which provide high recovery rate. For this purpose, cobalt(II/III) oxide@iron(II/III) oxide (Co₃O₄@Fe₃O₄) core–shell composite nanoflowers were fabricated via hydrothermal synthesis for the recovery of heavy metal ions (Pb²⁺ and Cd²⁺). X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometry (VSM) were used in the chemical and structural characterization of Co₃O₄@Fe₃O₄. Flame atomic absorption spectrometry (FAAS) was used for the determination of total metal content. In our work, optimum conditions for heavy metal on recovery such as eluent concentration, eluent type, pH, adsorbent amount, solution volume, sonication duration, were studied. As a result of these studies, quantitative recovery of analyte ions was obtained at pH 7.5. Quantitative recovery of Pb²⁺ ions was observed with 20 mL 1 M HNO₃ solution as eluent and 100 mg amount of adsorbent while, they were found for Cd²⁺ ion recovery with 5 mL 1 M HNO₃ solution as eluent and 200 mg amount of adsorbent. The highest recovery rates were found to be 99.6% and 99.9% for Pb²⁺ and Cd²⁺ heavy metal ions, respectively.

Keywords: Magnetic solid-phase extraction (MSPE); Co3O4@Fe3O4-doped nanoflowers; Flame atomic absorption spectrometry (FAAS)

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-024-03413-6

Chemical Papers 78 (7) 4495–4506 (2024)