Synthesis of mesoporous silica-coated magnetic nanoparticles modified with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole and its application as Cu(II) adsorbent from aqueous samples

Graphical abstract: - Highlights: • Groups of interest to perform metal complexation could be detected in the material. • Adsorption isotherms are in agreement with Langmuir model. • The material has a typical behavior of superparamagnetic material with high magnetization. - Abstract: This study presents an alternative, rapid, and environment-friendly synthesis procedure of a magnetic core–shell mesoporous SBA-15 silica composite, its functionalization with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole (Purpald), and its application in dispersive solid-phase microextraction (DSPME) for Cu(II) from water. The materials were characterized through magnetization measurements, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) of ²⁹Si and ¹³C, elemental analysis, and surface area measurements. FTIR and NMR analyses indicated the presence of the ligand on the functionalized material and that it was coupled through a C−S bond. TEM images clearly show that the magnetite core particles were effectively coated with a silica shell. The material presented a surface area of 287.99 m² g⁻¹ and an average pore diameter of approximately 15.1 nm. The material had its point of zero charge (PZC) determined (6.17) and its adsorption capacity was evaluated as a function of time, pH, and metal concentration. Dynamic adsorption equilibrium was reached in 120 min, and it had a good correlation with the pseudo-second-order kinetic model (r² = 0.9997). The maximum experimental adsorption capacity (0.0786 mmol g⁻¹) and the value calculated by the linearized Langmuir model (0.0799 mmol g⁻¹) are very approximate, indicating the formation of a monolayer over the material. Furthermore, the material proved to be very stable, because their adsorption capacity remained greater than 95% even after 10 cycles of adsorption/desorption. A high enrichment factor of 98.1-fold was observed, indicating that this material is suitable for the preconcentration of trace Cu(II) ions before analysis through flame atomic absorption spectrometry (FAAS).