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Preparation and characterization of metal-organic framework MIL-101(Cr)-coated solid-phase microextraction fiber.

Analytica chimica acta (2014-12-04)
Lijun Xie, Shuqin Liu, Zhubing Han, Ruifen Jiang, Hong Liu, Fang Zhu, Feng Zeng, Chengyong Su, Gangfeng Ouyang
ABSTRACT

Metal-organic frameworks (MOFs) have received great attention as novel sorbents due to their fascinating structures and intriguing potential applications in various fields. In this work, a MIL-101(Cr)-coated solid-phase microextraction (SPME) fiber was fabricated by a simple direct coating method and applied to the determination of volatile compounds (BTEX, benzene, toluene, ethylbenzene, m-xylene and o-xylene) and semi-volatile compounds (PAHs, polycyclic aromatic hydrocarbons) from water samples. The extraction and desorption conditions of headspace SPME (HS-SPME) were optimized. Under the optimized conditions, the established methods exhibited excellent extraction performance. Good precision (<7.7%) and low detection limits (0.32-1.7 ng L(-1) and 0.12-2.1 ng L(-1) for BTEX and PAHs, respectively) were achieved. In addition, the MIL-101(Cr)-coated fiber possessed good thermal stability, and the fiber can be reused over 150 times. The fiber was successfully applied to the analysis of BTEX and PAHs in river water by coupling with gas chromatography-mass spectrometry (GC-MS). The analytes at low concentrations (1.7 and 10 ng L(-1)) were detected, and the recoveries obtained with the spiked river water samples were in the range of 80.0-113% and 84.8-106% for BTEX and PAHs, respectively, which demonstrated the applicability of the self-made fiber.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ethylbenzene, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Benzene, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Sigma-Aldrich
o-Xylene, reagent grade, ≥98.0%
Sigma-Aldrich
Ethylbenzene, ReagentPlus®, 99%
Sigma-Aldrich
Toluene, Laboratory Reagent, ≥99.3%
Sigma-Aldrich
o-Xylene, puriss. p.a., ≥99.0% (GC)
Sigma-Aldrich
Benzene, puriss. p.a., reag. Ph. Eur., ≥99.7%
Sigma-Aldrich
Toluene, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.7% (GC)
Sigma-Aldrich
Benzene, ACS reagent, ≥99.0%
Supelco
SPME LC Tips, C18, tray of 96 ea
Supelco
o-Xylene, suitable for HPLC, 98%
Sigma-Aldrich
Toluene, suitable for HPLC, 99.9%
Sigma-Aldrich
Benzene, suitable for HPLC, ≥99.9%
Supelco
IonSense® PDMS/DVB SPE-it Tips, pkg of 96 ea
Supelco
o-Xylene, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), metal alloy fiber, for use with manual holder
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), for use with autosampler
Sigma-Aldrich
Toluene, anhydrous, 99.8%
Sigma-Aldrich
Ethylbenzene, anhydrous, 99.8%
Sigma-Aldrich
Benzene, anhydrous, 99.8%
Sigma-Aldrich
o-Xylene, anhydrous, 97%
Sigma-Aldrich
Benzene, ReagentPlus®, thiophene free, ≥99%
Supelco
SPME StableFlex fiber assortment kit, for use with autosampler, needle size 24 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 4, for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME fiber assortment kit 2, for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with manual holder