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Sulfite auto-oxidation catalyzed by cobalt complexed with ammonia deposited on silica (CoNSi) was used to generate sulfate radicals. The material was characterized by ATR–FTIR, suggesting that the silica structure did not change, and SEM–EDS, indicating an uniform dispersion of cobalt across the material surface according with XRD results. BET analysis provided information on a mesoporous material (type IV isotherm) with regular morphology (H1 hysteresis). The DSC analysis showed that CoNSi is thermally stable under the studied conditions. Quantitative analysis of Fipronil (FIP) was performed by HPLC-DAD, where the applied method was selective and linear. The Box–Behnken experimental design (BBD) method was used to define the best condition for removing the analyte in water. It was found that in 60 min, 76% removal of 1.8 mg L −1  of FIP was reached by adding 0.30 g of the material and 0.30 g of the sulfite in a solution under stirring, aeration, pH 8.0, and room temperature and protected from radiation. However, analysis of cobalt leaching into the solution by FAAS showed a small amount of the metal (0.44 mg L −1 ) informing that the synthesis of the material must be improved.

Removal of fipronil by advanced oxidative processes using sulfite activated by cobalt immobilized on silica