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  • Synthesis and characterization of composite polymer, polyethylene glycol grafted flower-like cupric nano oxide for solid phase microextraction of ultra-trace levels of benzene, toluene, ethyl benzene and o-xylene in human hair and water samples.

Synthesis and characterization of composite polymer, polyethylene glycol grafted flower-like cupric nano oxide for solid phase microextraction of ultra-trace levels of benzene, toluene, ethyl benzene and o-xylene in human hair and water samples.

Journal of chromatography. A (2015-09-29)
Ali Sarafraz-Yazdi, Amene Zendegi-Shiraz, Zarrin Es'haghi, Mohammad Hassanzadeh-Khayyat
ABSTRACT

In this research, poly (ethylene glycol)-poly (ethylene glycol) grafted flower-like cupric oxidenano particles (PEG-PEG-g-CuO NPs) as a novel fiber coating of solid-phase microextraction (SPME) were synthesized by using sol-gel technology. This fiber was successfully applied to extract and determine the ultra-trace levels of benzene, toluene, ethyl benzene and o-xylene in human hair using head space-solid-phase microextraction (HS-SPME) coupled to gas chromatography-flame ionization detector. Characterization and chemical composition of the nano particle was performed by Fourier transform infrared spectroscopy (FT-IR), energy dispersion spectroscopy (EDS) and back scatter analysis (BSA). These methods confirmed the successful fabrication of PEG-g-CuO NPs. The surface morphology of the fibers were inspected by scanning electron microscopy. The scanning electron microscopy (SEM) revealed many "crack-like" features and highly porous structure on the surface of fiber. The synthesized nanocomposites were used for preconcentration and extraction of benzene, toluene, ethyl benzene and o-xylene (BTEX). The effects of operating parameters such as: desorption temperature and time, extraction temperature, extraction time, stirring speed and salt effect were investigated and optimized. Under the optimal conditions, the method detection limits and the limits of quantification were between 0.00025-50.00000pgmL(-1) and 0.00200-200.00000pgmL(-1), respectively. Linearity was observed over a range 0.00200-200000.00000pgmL(-1). The relative standard deviations for one fiber (repeatability; n=5) were obtained from 3.30 up to 5.01% and between fibers or batch to batch (n=3; reproducibility) in the range of 3.63-6.21%. The developed method was successfully applied to simultaneous determination of BTEX in human hairs, tap water and distillate water.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME Portable Field Sampler, coating CAR/PDMS
Supelco
SPME Fiber Assembly, 7 μm PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, green hub
Supelco
SPME Sampling Stand, for use with 15 mL vials
Sigma-Aldrich
Acetone, ≥99%, FCC, FG
Sigma-Aldrich
Acetone, natural, ≥97%
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, blue hub
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub
Supelco
SPME Fiber Assembly, 30 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, yellow hub
Supelco
SPME Fiber Assembly, 85 μm Polyacrylate, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, white hub
Supelco
SPME Fiber Assembly, 30 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, yellow hub
Supelco
SPME Fiber Assembly, 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, red hub
Supelco
SPME Fiber Assembly, 7 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, green hub
Supelco
SPME Fiber Assembly, 7 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, green hub
Supelco
SPME Fiber Assembly, 100 μm PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, red hub
Sigma-Aldrich
Sodium chloride-35Cl, 99 atom % 35Cl
Sigma-Aldrich
Sodium chloride, random crystals, 99.9% trace metals basis
Supelco
SPME Portable Field Sampler, coating PDMS
Supelco
SPME Fiber Assembly, 85 μm Polyacrylate, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, white hub
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, blue hub
Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of, plain gray hub
Sigma-Aldrich
Sodium chloride, tablet
Sigma-Aldrich
Sodium chloride, AnhydroBeads, −10 mesh, 99.999% trace metals basis
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Supelco
SPME Fiber Assembly, 60 μm PEG, Metal Alloy (1 cm), needle size 23 ga, Manual Holder, pk of 3, purple hub
Supelco
SPME Fiber Assembly, 100 μm PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, red hub
SAFC
Sodium chloride solution, 5 M
Sigma-Aldrich
Methanol, purification grade, 99.8%