| Summary: | In this study, Chalcopyrite (CuFeS<sub>2</sub>) was prepared by a hydrothermal and co-precipitation method, being represented as H-CuFeS<sub>2</sub> and C-CuFeS<sub>2</sub>, respectively. The prepared CuFeS<sub>2</sub> samples were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy mapping (EDS-mapping), powder X-ray diffractometer (XRD), X-ray photoelectron spectrometry (XPS), and Raman microscope. Rhodamine B (RhB, 20 ppm) was used as the target pollutant to evaluate the degradation performance by the prepared CuFeS<sub>2</sub> samples. The H-CuFeS<sub>2</sub> samples (20 mg) in the presence of Na<sub>2</sub>S<sub>2</sub>O<sub>8</sub> (4 mM) exhibited excellent degradation efficiency (98.8% within 10 min). Through free radical trapping experiment, the major active species were •SO<sub>4</sub><sup>−</sup> radicals and •OH radicals involved the RhB degradation. Furthermore, •SO<sub>4</sub><sup>−</sup> radicals produced from the prepared samples were evaluated by iodometric titration. In addition, one possible degradation mechanism was proposed. Finally, the prepared H-CuFeS<sub>2</sub> samples were used to degrade different dyestuff (rhodamine 6G, methylene blue, and methyl orange) and organic pollutant (bisphenol A) in the different environmental water samples (pond water and seawater) with 10.1% mineral efficiency improvement comparing to traditional Fenton reaction.
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