Abstract
The accurate determination of trace metals in aqueous matrices necessitates robust sample preparation techniques that enable selective preconcentration of analytes while ensuring compatibility with subsequent instrumental analysis. Dispersive solid-phase extraction (d-SPE), a suspension-based variant of conventional solid-phase extraction (SPE), facilitates rapid sorbent-analyte interactions and enhances mass transfer efficiency through direct dispersion of the sorbent in the sample solution. This approach offers significant advantages over traditional column-based SPE, including faster extraction kinetics and greater operational simplicity. When supported by appropriately engineered sorbents, d-SPE exhibits considerable potential for the selective enrichment of trace metal analytes from complex aqueous matrices. In this work, a fibrous silica-based chelating material, DSA-KCC-1, was synthesized by grafting 3,5-Di-tert-butylsalicylaldehyde (DSA) onto aminopropyl-modified KCC-1. The dendritic KCC-1 scaffold enables fast dispersion and short diffusion pathways, while the immobilized phenolate-imine ligand introduces defined binding sites for transition-metal uptake. Characterization by FTIR, TGA, BET, FESEM/TEM, XRD, and elemental analysis confirmed the successfulness of functionalization and preservation of the fibrous mesostructured. Adsorption studies demonstrated chemisorption-driven interactions for Pb(II) and Co(II) from water, with Langmuir-type monolayer uptake and pseudo-second-order kinetic behavior. The nano-adsorbent exhibited a markedly higher affinity for Pb(II) than for Co(II), with maximum adsorption capacities of 99.73 and 66.26 mg g(-1), respectively. Integration of the DSA-KCC-1 nanosorbent into a d-SPE-ICP-OES workflow enabled the reliable determination of trace levels of the target ions, delivering low limits of detection, wide linear calibration ranges, and stable performance over repeated extraction cycles. Analysis of NIST CRM 1643d yielded results in good agreement with the certified values, while the method demonstrated high tolerance toward common coexisting ions. The combined structural features of the KCC-1 support and the Schiff-base ligand indicate the suitability of DSA-KCC-1 for d-SPE workflows and demonstrate the potential of this SPE format for selective preconcentration of trace metal ions in aqueous matrices.