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  • Needle trap micro-extraction for VOC analysis: effects of packing materials and desorption parameters.

Needle trap micro-extraction for VOC analysis: effects of packing materials and desorption parameters.

Journal of chromatography. A (2011-12-06)
Phillip Trefz, Sabine Kischkel, Dietmar Hein, Ellwood Sean James, Jochen K Schubert, Wolfram Miekisch
ABSTRACT

Combining advantages of SPE and SPME needle trap devices (NTD) represent promising new tools for a robust and reproducible sample preparation. This study was intended to investigate the effect of different packing materials on efficacy and reproducibility of VOC analysis by means of needle trap micro extraction (NTME). NTDs with a side hole design and containing different combinations of PDMS, DVB and Carbopack X and Carboxen 1000 and NTDs containing a single layer organic polymer of methacrylic acid and ethylene glycol dimethacrylate were investigated with respect to reproducibility, LODs and LOQs, carry over and storage. NTDs were loaded with VOC standard gas mixtures containing saturated and unsaturated hydrocarbons, oxygenated and aromatic compounds. Volatile substances were thermally desorbed from the NTDs using fast expansive flow technique and separated, identified and quantified by means of GC-MS. Optimal desorption temperatures between 200 and 290°C could be identified for the different types of NTDs with respect to desorption efficiency and variation. Carry over was below 6% for polymer packed needles and up to 67% in PDMS/Carboxen 1000 NTDs. Intra and inter needle variation was best for polymer NTDs and consistently below 9% for this type of NTD. LODs and LOQs were in the range of some ng/L. Sensitivity of the method could be improved by increasing sample volume. NTDs packed with a copolymer of methacrylic acid and ethylene glycol dimethacrylate were universally applicable for sample preparation in VOC analysis. If aromatic compounds were to be determined DVB/Carboxen 1000 and DVB/Carbopack X/Carboxen 1000 devices could be considered as an alternative. PDMS/Carbopack X/Carboxen 1000 NTDs may represent a good alternative for the analysis of hydrocarbons and aldehydes. NTME represents a powerful tool for different application areas, from environmental monitoring to breath analysis.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
Supelco
Carbopack B, stainless steel TD tube, O.D. × L 1/4 × 3 1/2, unconditioned, pkg of 10 ea
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
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., unconditioned, pkg of 10 ea, matrix Carbopack
Sigma-Aldrich
Divinylbenzene, technical grade, 55%
Sigma-Aldrich
Divinylbenzene, technical grade, 80%
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Carbopack Adsorbent, matrix Carbopack X, 60-80 mesh, bottle of 10 g
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack X, 120-400 mesh, bottle of 50 g
Supelco
Carbopack Adsorbent, matrix Carbopack C, 60-80 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack C, 80-100 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, pack of 144 × 290 mg
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm