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  • Critical role of a pre-purge setup in the thermal desorption analysis of volatile organic compounds by gas chromatography with mass spectrometry.

Critical role of a pre-purge setup in the thermal desorption analysis of volatile organic compounds by gas chromatography with mass spectrometry.

Journal of separation science (2015-05-12)
Yong-Hyun Kim, Ki-Hyun Kim
ABSTRACT

In general, volatile organic compounds in ambient air are quantified by following a well-defined standard calibration procedure using a gas-/liquid-phase standard. If the liquid standard is analyzed by a thermal desorption, the solvent effect is unavoidable through the alteration of breakthrough properties or retention times. To learn more about the variables of the thermal desorption-based analysis, the effect of pre-purge conditions was evaluated for 18 volatile organic compounds with different types of sorbent tube materials by fixing standard volume (1 μL) and flow rate (100 mL/min). The gas phase calibration was also carried out as reference for the non-solvent effect. A single tube filled with Tenax TA exhibited the least solvent effect with the short pre-purge (1 min), while being subject to the breakthrough at or above 10 min pre-purge. For a three-bed sorbent tube with Carboxen 1000, at least 10 min of pre-purge was needed for the compounds with a retention time close to methanol (e.g., propanal). Another three-bed tube with Carbopack X reduced the solvent effect efficiently for a short pre-purge (2 min) without the breakthrough. As such, the solvent effect can be adjusted by the proper control of the sorbent tube application.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray 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
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carbopack Adsorbent, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack C, 80-100 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
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, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray 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
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carbopack Adsorbent, matrix Carbopack C, 60-80 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 × 0.53 mm, average thickness 30 μm
Supelco
Carbopack Adsorbent, matrix Carbopack X, 120-400 mesh, bottle of 50 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Sigma-Aldrich
4-Methyl-2-pentanone, ≥99%, FCC
Sigma-Aldrich
Palmitoylethanolamide
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., unconditioned, pkg of 10 ea, matrix Carbopack
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
Supelco
Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of, plain gray hub
Supelco
SPME Fiber Assembly, 85 μm CAR/PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, light blue hub
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g