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  • Simultaneous determination of 76 micropollutants in water samples by headspace solid phase microextraction and gas chromatography-mass spectrometry.

Simultaneous determination of 76 micropollutants in water samples by headspace solid phase microextraction and gas chromatography-mass spectrometry.

Talanta (2013-10-24)
C Martínez, N Ramírez, V Gómez, E Pocurull, F Borrull
ABSTRACT

This study focuses on the development of an analytical method based on headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of 76 micropollutants in water samples. The selected micropollutants include volatile organic compounds (VOCs) (e.g. chlorobenzenes, chloroalkanes), endocrine disrupting compounds (EDCs) (e.g. bisphenol A and tributyl phosphate), odour compounds (e.g. limonene, phenol), fragrance allergens (e.g. geraniol, eugenol) and some pesticides (e.g. heptachlor, terbutryn). The experimental conditions affecting their extraction, such as the type of fibre, temperature and time of extraction, sample volume and ionic strength of the samples were optimized using HS-SPME. The method showed good linear range, reproducibility between days, repeatability and low detection limits (at ng L(-1) levels). The validated method has been applied to determine the target organic micropollutants in aqueous samples from different experimental research units of surface water, sea water, waste water and those effluents of advance membrane treatments. The optimized method showed good performance in the different types of samples studied. The analysis revealed the presence of several micropollutants at concentrations between 20 and 5000 μg L(-1), such as ethylbenzene, o-xylene, p-isopropilbenzene, D-limonene, citral and isoeugenol, due to the fact that these species are commonly used in domestic and industrial applications.

MATERIALS
Product Number
Brand
Product Description

Supelco
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, black hub
Supelco
SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
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, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, pack of 144 × 290 mg
Supelco
SPME Fiber Assembly, 85 μm CAR/PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, light blue hub
Supelco
Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
Supelco
ORBO-93 Sorbent Tube, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
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Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
Sigma-Aldrich
Tributyl phosphate, 97%
Supelco
ORBO 90 Carboxen® 564 (20/45), 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
Supelco
ORBO 78 HBr on Carboxen® 564 specially cleaned (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea