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Merck
  • 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
摘要

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.

材料
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产品描述

Sigma-Aldrich
二乙烯基苯, technical grade, 80%
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), needle size 24 ga, StableFlex fiber, for use with autosampler, fiber L 2 cm, pk of 3
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler, fiber L 1 cm, pk of 3
Supelco
ORBO Carboxen-564 管, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler, fiber L 1 cm, pk of 3
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler, fiber L 2 cm, pk of 3
Supelco
ORBO-78 400/200mg,每包 25 支, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
Carboxen®1010 多孔层壁涂开管柱, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Sigma-Aldrich
二乙烯基苯, technical grade, 55%
Supelco
Carbopack®吸附剂, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
FLM Carbopack X去活不锈钢TD管, preconditioned, pkg of 10 tubes, O.D. × L 1/4 in. (6.35 mm) × 3 1/2 in. (89 mm)
Supelco
Carboxen® 1006 多孔层壁涂开管柱, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
Supelco
Carboxen®1010 多孔层壁涂开管柱, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carbopack吸附剂, matrix Carbopack B, 60-80 mesh, bottle of 10 g
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
Carbopack吸附剂, matrix Carbopack C, 80-100 mesh, bottle of 10 g
Supelco
Carbopack吸附剂, matrix Carbopack C, 60-80 mesh, bottle of 10 g
Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Carboxen® 1006 多孔层壁涂开管柱, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carbopack吸附剂, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
Supelco
Carboxen® 1000 双向固相萃取管, 200 mg/mL, pk 30
Supelco
Carbopack®吸附剂, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
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