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Merck

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
RESUMEN

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.

MATERIALES
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Sigma-Aldrich
Divinylbenzene, technical grade, 80%
Supelco
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
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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, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
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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®-1010 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 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Sigma-Aldrich
Divinylbenzene, technical grade, 55%
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Tubo TD de acero inoxidable desactivado FLM Carbopack X, preconditioned, pkg of 10 tubes, O.D. × L 1/4 in. (6.35 mm) × 3 1/2 in. (89 mm)
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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 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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Adsorbente Carbopack, matrix Carbopack B, 60-80 mesh, bottle of 10 g
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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, for use with manual holder, StableFlex fiber
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
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Adsorbente Carbopack, matrix Carbopack C, 80-100 mesh, bottle of 10 g
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Adsorbente Carbopack, matrix Carbopack C, 60-80 mesh, bottle of 10 g
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
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Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Adsorbente Carbopack, matrix Carbopack X, 40-60 mesh, bottle of 10 g
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, 50/30µm DVB/CAR/PDMS, Metal Alloy (2cm), needle size 23 ga, Autosampler, pk of 1 ×, plain gray hub
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Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
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Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
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Carbopack B, O.D. × L 1/4 in. × 3 1/2 in., glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea