<p>Polyimide (PI) and multi-walled carbon nanotube (MWCNT) composite solid-phase microextraction (SPME) fibers were prepared for headspace SPME (HS-SPME) and combined with thermal desorption and gas chromatography-flame ionization detection (TD-GC-FID) for the analysis of benzene, toluene, ethylbenzene, and xylene (BTEX) in water. The MWCNT/PI dispersion DMF solution was dip-coated and instantly solidified via phase inversion in water. The incorporation of MWCNTs was confirmed by FT-IR and elemental mapping. Surface open large pores of ~ 500&#xa0;nm and the abundant mesopores of ~ 5&#xa0;nm within the fiber were revealed by SEM and BET. It was found that the MWCNT/PI SPME fiber exhibited excellent thermal stability, with decomposition initiating at over 400&#xa0;°C, which is higher than those of MWCNTs or PI alone. The MWCNT/PI HS-SPME/TD-GC-FID method was established and demonstrated a wide linear range (5–500&#xa0;ng&#xa0;mL<sup>−1</sup>), good precision (with intra and inter-day RSDs ranging from 2.93 to 6.58% and 3.07 to 5.37%, respectively), low LODs (0.286–2.583&#xa0;ng&#xa0;mL<sup>−1</sup>), and high fiber-to-fiber reproducibility (RSDs between 3.00 and 5.15%). Finally, the method was applied to determine BTEX in real water samples. The relative recoveries were between 83.8 and 122% with standard deviations between 1.8 and 9.9%. These results indicate that MWCNT/PI is a facile, reliable, and high-efficient extraction phase for SPME, especially for the determination of BTEX in water.</p>

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High-Temperature Resistant MWCNT/Polyimide SPME Fiber Coupled with Thermal Desorption-GC for Determination of BTEX in Environmental Water

  • Chenglong Shi,
  • Xiaohui Yan,
  • Zhipeng Zhu,
  • Min Zhang,
  • Cheng Chen,
  • Hongxing Liu,
  • Dapeng Wu

摘要

Polyimide (PI) and multi-walled carbon nanotube (MWCNT) composite solid-phase microextraction (SPME) fibers were prepared for headspace SPME (HS-SPME) and combined with thermal desorption and gas chromatography-flame ionization detection (TD-GC-FID) for the analysis of benzene, toluene, ethylbenzene, and xylene (BTEX) in water. The MWCNT/PI dispersion DMF solution was dip-coated and instantly solidified via phase inversion in water. The incorporation of MWCNTs was confirmed by FT-IR and elemental mapping. Surface open large pores of ~ 500 nm and the abundant mesopores of ~ 5 nm within the fiber were revealed by SEM and BET. It was found that the MWCNT/PI SPME fiber exhibited excellent thermal stability, with decomposition initiating at over 400 °C, which is higher than those of MWCNTs or PI alone. The MWCNT/PI HS-SPME/TD-GC-FID method was established and demonstrated a wide linear range (5–500 ng mL−1), good precision (with intra and inter-day RSDs ranging from 2.93 to 6.58% and 3.07 to 5.37%, respectively), low LODs (0.286–2.583 ng mL−1), and high fiber-to-fiber reproducibility (RSDs between 3.00 and 5.15%). Finally, the method was applied to determine BTEX in real water samples. The relative recoveries were between 83.8 and 122% with standard deviations between 1.8 and 9.9%. These results indicate that MWCNT/PI is a facile, reliable, and high-efficient extraction phase for SPME, especially for the determination of BTEX in water.