Fabrication of Lead‐based Metal‐Organic Frameworks Using Recovered Lead for Solid‐Phase Microextraction of p ‐Phenylenediamine Antioxidants

ABSTRACT

The recycling of waste lead‐acid batteries and the sensitive detection of trace p ‐phenylenediamine (PPD) antioxidants represent two pressing challenges in resource recovery and environmental safety. Herein, an integrated solution was proposed by synthesizing a novel lead‐based metal‐organic framework (WLP‐Pb‐MOF) from waste lead paste (WLP) as a sustainable metal source. The material served as a coating for a solid‐phase microextraction (SPME) fiber. When coupled with gas chromatography‐mass spectrometry, it enabled a highly sensitive method for determining three PPDs in water samples. The unique slit‐shaped pore architecture and hydrophobic surface of WLP‐Pb‐MOF facilitated efficient enrichment through synergistic interactions, including size‐sieving, hydrophobic partitioning, π‐π stacking, and hydrogen bonding. This synergy resulted in extraction efficiencies significantly outperforming commercial SPME fibers. The method demonstrated good linearity from 5 to 2000 ng L ⁻¹ , with detection limits of 0.29–1.60 ng L ⁻¹ . In real water samples, the method achieved spiked recoveries of 91.3%–108.5%, with relative standard deviations below 8.78%. These results confirmed its accuracy and practical reliability. This work not only presents a viable strategy for the value‐added recycling of waste lead but also provides a robust analytical platform for monitoring trace organic pollutants, effectively bridging sustainable resource recovery with advanced environmental monitoring.