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Merck

Determination of ethylene oxide by solid-phase microextraction device with on-fiber derivatization.

Journal of chromatography. A (2003-04-22)
Shih-Wei Tsai, Kai-Kuang Wu
RESUMEN

The solid-phase microextraction (SPME) device was used as a time-weighted average (TWA) sampler for ethylene oxide. Carboxen/polydimethylsiloxane (CAR/PDMS) fiber was used and hydrogen bromide (HBr) was loaded onto the fiber. The SPME fiber assembly was then inserted into PTFE tubing to improve the wearer's acceptance as a diffusive sampler. Known concentrations of ethylene oxide around the threshold limit values (TLVs)/time-weighted average and specific relative humidities (RHs) were generated by syringe pumps in a dynamic generation system. Ethylene oxide in gas bags were also generated. An exposure chamber was designed to allow measurement of face velocities, temperatures, exposing vapor concentrations, and RHs. Gas chromatography-mass spectrometry (GC-MS) was used for sample analysis. The appropriate adsorption time for SPME coating HBr was found to be 30 s and the desorption time for 2-bromothanol formed after sampling was determined to be 5 min. The experimental sampling constant of the sampler was found to be (2.96 +/- 0.09) x 10(-2) cm3/min, while face velocity (0-0.25 m/s) as well as RHs (10-80%) were not expected to have effects on the sampler.

MATERIALES
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Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, for use with manual holder
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with autosampler
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
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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)
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex, for use with autosampler
Sigma-Aldrich
2-Bromoethanol, 95%
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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ORBO-78 400/200 MG PK/25, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
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Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
2-Bromoethanol, analytical standard
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
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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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Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
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Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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Tubo absorbente ORBO-93, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm