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Semiconductor Zn-based nanomaterials have emerged as promising agents for the photocatalytic degradation of organic pollutants in wastewater treatment. However, achieving efficient synthesis protocols capable of rapidly producing small structures directly in aqueous environments remains challenging. Microwave-assisted synthesis presents a viable solution by enabling one-step particle generation swiftly and directly in water through increased pressure, thereby easily elevating the boiling point. This study investigates the microwave-assisted one-step synthesis of pure and iron-doped ZnS nanoparticles and assesses their efficacy in photodegrading Quinoline Yellow (QY) in aqueous suspensions. The results demonstrate a significant degradation of QY in the presence of 1% iron-doped ZnS nanoparticles, achieving approximately 66.3% degradation with 500 ppm of doped nanoparticles after 270 min. These findings highlight the considerable potential of 1% iron-doped ZnS nanoparticles as effective nanocatalysts.