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Merck
  • Development of SPME on-fiber derivatization for the sampling of formaldehyde and other carbonyl compounds in indoor air.

Development of SPME on-fiber derivatization for the sampling of formaldehyde and other carbonyl compounds in indoor air.

Analytical and bioanalytical chemistry (2013-11-21)
Delphine Bourdin, Valérie Desauziers
摘要

Solid-phase microextraction on-fiber derivatization applied to carbonyl compounds is known, but application to indoor air is poorly developed and the methods deserve to be complemented and optimized. In this work, two derivatization reagents, pentafluorophenylhydrazine and o-2,3,4,5,6-(pentaflurobenzyl)hydroxylamine (PFBHA), and three fiber coatings were tested in order to select the best combination. As Carboxen-based coatings were proven to induce the formation of by-products during the thermal desorption step, a polydimethylsiloxane-divinylbenzene fiber in association with PFBHA was finally chosen. The study of the derivatization kinetics showed that the reaction of PFBHA with carbonyl compounds was instantaneous, except for acetone. Analyses were performed by gas chromatography coupled with flame ionization detection and mass spectrometry. For 5 min fiber exposure, the limits of detection are below 0.5 μg m(-3) in selected ion monitoring mode, the reproducibility was 15% on average, and the linearity of the calibration curves was satisfactory. For on-site application, the influence of air humidity and the conditions in which the impregnated fibers were stored were studied. It is possible to store the fibers for 3 days before and for at least 2 days after sampling. The relative humidity of air was shown to have no influence on solid-phase microextraction sampling in the range from 0 to 70%. For formaldehyde, the method was compared with sampling on 2,4-dinitrophenylhydrazine cartridges, and the first results showed good agreement. Finally, the method was applied to three different indoor environments to check its feasibility.

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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
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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
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Carboxen® 1006 多孔层壁涂开管柱, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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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
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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
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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
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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
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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
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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
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