Nano-structured lead dioxide as a novel stationary phase for solid-phase microextraction

Area of Science:

• Analytical Chemistry
• Materials Science
• Environmental Science

Background:

• Solid-phase microextraction (SPME) is a widely used technique for sample preparation.
• Development of novel, efficient, and cost-effective SPME fibers is crucial for trace analysis.
• Lead dioxide (PbO2) has not been previously explored as a material for SPME fibers.

Purpose of the Study:

• To investigate the efficacy of nano-structured lead dioxide (PbO2) as a novel fiber material for SPME.
• To evaluate the extraction performance of PbO2 fibers for volatile organic compounds, specifically benzene, toluene, ethylbenzene, and xylenes (BTEX).
• To optimize the headspace solid-phase microextraction (HS-SPME) method using PbO2 fibers and assess its suitability for environmental water analysis.

Main Methods:

• Fabrication of nano-structured lead dioxide (PbO2) fibers via electrochemical deposition on platinum wire.
• Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-flame ionization detection (GC-FID).
• Optimization of extraction parameters: coating preparation, salt concentration, adsorption/desorption time and temperature, and stirring rate.

Main Results:

• PbO2 fibers exhibited high efficiency for the extraction of BTEX compounds from aqueous samples.
• Linear calibration curves (R2 > 0.994) were achieved in the concentration range of 0.1-100 µg L⁻¹, with detection limits below 0.012 µg L⁻¹.
• The PbO2 fibers demonstrated excellent thermal stability (up to 300°C), high extraction capacity, long lifespan (>50 uses), good repeatability (<10.0%), and reproducibility (<12.5%), with recoveries of 81-108% for environmental samples.

Conclusions:

• Nano-structured lead dioxide (PbO2) is a promising and efficient material for developing new SPME fibers.
• PbO2-based SPME fibers offer advantages such as high stability, capacity, reusability, chemical resistance, and lower cost compared to commercial alternatives.
• The developed HS-SPME method using PbO2 fibers is suitable for the reliable and sensitive analysis of BTEX in environmental water samples.