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Merck

Trace determination of volatile sulfur compounds by solid-phase microextraction and GC-MS.

The Analyst (2002-08-28)
Annika T Nielsen, Susanne Jonsson
RESUMO

A method was developed for the simultaneous determination of the following nine volatile sulfur compounds in gas samples: carbon disulfide, carbonyl sulfide, ethyl sulfide, ethyl methyl sulfide, hydrogen sulfide, isopropanethiol, methanethiol, methyl disulfide and methyl sulfide. The target compounds were preconcentrated by solid-phase microextraction (SPME) and determined by gas chromatography combined with mass spectrometry. Experimental design was employed to optimize the extraction time and temperature and concurrent detection of the nine compounds was achieved by using an SPME fiber coated with Carboxen-polydimethylsiloxane (75 microns). Detection limits ranged from 1 ppt (v/v) for carbon disulfide to 350 ppt (v/v) for hydrogen sulfide and calibration functions were linear up to 20 ppb (v/v) for all the compounds investigated.

MATERIAIS
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Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), needle size 24 ga, StableFlex
Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), 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)
Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Supelco
Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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Adsorvente Carboxen®, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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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
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Coluna de GC capilar Carboxen®-1006 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
Conjunto de fibras de SPME Carboxeno/polidimetilsiloxano (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Coluna de GC capilar Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Adsorvente Carboxen®, 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
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Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
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Adsorvente Carboxen®, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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Adsorvente Carboxen®, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
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Adsorvente Carboxen®, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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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
Supelco
Conjunto de fibras para SPME de divinilbenzeno-carboxeno-polidimetilsiloxano (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
Supelco
Adsorvente Carboxen®, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
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Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea