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

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

The Analyst (2002-08-28)

Annika T Nielsen, Susanne Jonsson

PMID12195944

ABSTRACT

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.

MATERIALS

Product Number

Brand

Product Description

20358

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)

28718-U

Supelco

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

29534-U

Supelco

Carboxen^® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea

20355

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

25467

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

24246

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

10478-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 60-80 mesh, bottle of 10 g

24241-U

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

25461

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

57328-U

Supelco

SPME Fiber Assembly, matrix active group 50/30µm DVB/CAR/PDMS, StableFlex fiber, manual holder, needle size 24 ga

57298-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub

57343-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler

57295-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler

57318

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga

57914-U

Supelco

SPME Fiber Assembly, for use with autosampler, matrix active group 50/30µm DVB/CAR/PDMS, needle size 23 ga, metal alloy fiber, fiber L 2 cm

57319

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler

57906-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber

57912-U

Supelco

SPME Fiber Assembly, matrix active group 50/30µm DVB/CAR/PDMS, needle size 23 ga, metal alloy fiber, for use with autosampler, fiber L 1 cm, pkg of 1 × ea

57329-U

Supelco

SPME Fiber Assembly, matrix active group 50/30µm DVB/CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler, fiber L 1 cm, pk of 3

57335-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler

57334-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber

57344-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder

57299-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub

57348-U

Supelco

SPME Fiber Assembly, matrix active group 50/30µm DVB/CAR/PDMS, needle size 24 ga, StableFlex fiber, for use with autosampler, fiber L 2 cm, pk of 3

54041-U

Supelco

Carboxen^® 1000 Reversible SPE Tube, 200 mg/mL, pk 30

54294-U

Supelco

Carboxen^® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea

23446-U

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