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A straightforward, fast and efficient analytical method was developed which utilizes a magnetic composite called three-dimensional graphene (3D-G@Fe3O4) as an adsorbent to recover nitrite ions (NO2−) from environmental water samples. The investigation into the synthesized adsorbent contained an examination of its morphology, chemical composition, structural attributes, and magnetic properties. This comprehensive analysis was conducted using various instrumental techniques, including Fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Raman spectroscopy, X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), Barrett-Joyner-Halenda (BJH), and vibrating sample magnetometry (VSM). The adsorbent surface was activated by adding cetyltrimethylammonium bromide (CTAB) to the sample solution. To improve the selectivity and sensitivity of the method, nitrite ions were reacted with sulfanilic acid and chromotropic acid sequentially. An orange-red azo-dye complex was formed in the presence of nitrite ions with a clear absorbance peak at 514 nm. The effect of the main experimental parameters such as the pH of the sample solution, adsorbent dosage, and CTAB dosage was explored, and the optimization process was performed using a central composite design (CCD). The linear dynamic range (20–100 ng mL−1) was determined under optimal experimental circumstances, yielding a reasonable determination coefficient (R2, 0.9993), a detection limit of 5.12 ng mL−1, an enrichment factor of 167, and precision values of 1.0% intraday and 2.9% inter-day. The methodology successfully identified minute nitrite ions in environmental water samples with relative recoveries that varied between 96.05 and 101.6 ng mL−1. [ABSTRACT FROM AUTHOR]