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  • Development and validation of a method for air-quality and nuisance odors monitoring of volatile organic compounds using multi-sorbent adsorption and gas chromatography/mass spectrometry thermal desorption system.

Development and validation of a method for air-quality and nuisance odors monitoring of volatile organic compounds using multi-sorbent adsorption and gas chromatography/mass spectrometry thermal desorption system.

Journal of chromatography. A (2006-12-26)
Alejandra Ribes, Guillem Carrera, Eva Gallego, Xavier Roca, M A José Berenguer, Xavier Guardino
ABSTRACT

An analytical method based on thermal desorption (TD) coupled to gas chromatography (GC) and mass spectrometry detection (MS) has been developed and validated for the determination of a wide range of odor nuisance and air-quality volatile organic compounds (VOC) in air. New generation isocyanates, isocyanato- and isothiocyanatocyclohexane, have been included for the first time as target compounds due to their high occurrence in air samples. A dynamic air sampling method to trap gas and vapor on multi-sorbent tubes using portable pump equipment has been also developed. Sorbent tubes were filled with Carbotrap (70mg), Carbopack X (100mg) and Carboxen-569 (90mg). Validation of the TD-GC-MS method showed good selectivity, sensibility and precision according to Compendium Method TO-17 (US Environment Protection Agency) criteria. Limits of detection (signal-to-noise=3, ng in tube) ranges were 0.004-0.03ng (alcanes), 0.001-0.1ng (aromatics), 0.03-14ng (aldehydes), 0.003-7ng (alcohols), 0.003-0.04ng (chlorides), 0.02-0.5ng (esters), 0.002-0.1ng (ketones), 0.01-0.53ng (terpenes), 14-97ng (amides), 0.2-10ng (isocyanates) and 0.001ng (carbon disulfide). The linear dynamic range was over 3-5 orders of magnitude, depending of the VOC. TD-GC-MS analysis was reproducible, with relative standard deviation (n=5) within 20%. VOCs breakthrough examination showed no significant losses when about 2000ng standard was prepared. In order to evaluate the performance of the developed method on real samples, several industrial and urban air samples were analysed. VOCs were found to be stable on the sorbent tubes for at least 1 week when stored at 4 degrees C.

MATERIALI
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Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
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
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Adsorbente Carboxen®, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
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Colonna capillare per GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub
Supelco
FLM Carbopack X Deactivated Stainless Steel TD Tube, preconditioned, pkg of 10 tubes, O.D. × L 1/4 in. (6.35 mm) × 3 1/2 in. (89 mm)
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Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Carbopack Adsorbent, matrix Carbopack B, 60-80 mesh, bottle of 10 g
Supelco
Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub
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Carbotrap® Adsorbent, matrix Carbotrap® B, 20-40 mesh, bottle of 10 g
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Carbopack Adsorbent, matrix Carbopack C, 80-100 mesh, bottle of 10 g
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub
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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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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub
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Carbotrap® 300, O.D. × L 1/4 in. × 3 1/2 in., glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea
Supelco
Carbopack Adsorbent, matrix Carbopack C, 60-80 mesh, bottle of 10 g
Supelco
Carbotrap® 300, O.D. × L 1/4 in. × 3 1/2 in., stainless steel TD tube, preconditioned, pkg of 10 ea
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Colonna capillare per GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Tenax® TA / Carboxen® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok® End-Fittings), pkg of 10 ea
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, black hub
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Carbopack Adsorbent, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
Adsorbente Carboxen®, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g