Synthesis of a Hematite-Geopolymer Composite: Optimization of Formulation Parameters and Application to the Detection of Pb2+ Ions in Aqueous Solution

Abstract

The Composite Centered Experimental Design (CCED) using the response surface methodology was used to optimize the synthesis of a hematite-geopolymer composite, applied to the preparation of a Pb²⁺ electrochemical sensor. Two important experimental parameters in the formulation (curing time and hematite content) were considered in the optimization of the synthesis of the composite material. The electrochemical signal of Pb²⁺ at a carbon paste electrode modified by the synthesized composite was used as a response to identify the best formulation. After applying the generated experimental plan, the optimal composite material was obtained using 17.08% hematite and a curing time of 0.16 days. The characterization of the optimized composite material revealed the presence of a porous structure and a poly(phospho-ferro-siloxo) network, but with a fraction of well dispersed and unreacted hematite. Preliminary experiments confirmed that the sensor prepared with the composite showed high stability and reproducibility of the Pb (II) signal, justifying its application for accurate sensing of the metal cation in an aqueous solution. A Pb²⁺ calibration curve was obtained after optimizing the experimental detection parameters (composition of the carbon paste electrode, pH of the accumulation solution, accumulation time, and electrolysis potential). A detection limit of 0.2 nM (based on a signal-to-noise ratio of 3) was obtained for a studied concentration range between 0.04 and 0.48 nM. The designed sensor also showed remarkable selectivity and excellent performance in real media samples (spring, tap, rain, and well water).