RESUMO
Samplers for VOCs in air based on cyclodextrin-silica hybrid microporous solid phases are proposed. The solid phase preparation is very easy and inexpensive. Proposed samplers compared with other solid phases present the advantages of a wider range of operative conditions for VOCs desorption. Samplers are tested based on results for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene (BTEX) in air. Operational parameters are optimized and quantitative recovery is obtained using a solid phase from 2-hydroxypropyl-ß-cyclodextrin and acetonitrile as the extraction solvent. The recoveries obtained are 89 ± 4%, 90 ± 6%, 91 ± 2%, 87.0 ± 0.9%, 88 ± 4%, and 88 ± 4% for benzene, toluene, ethylbenzene, o-xylene, m-xylene and p-xylene, respectively. Moreover results indicate a good reproducibility with a coefficient of variation below 6% and no significant difference between the reproducibility intra-synthesis and inter-synthesis. The proposed procedure has been applied to the determination of BTEX in several contaminated air samples and compared with results provided by a reference method.
RESUMO
An HPLC method for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene in occupational environments was developed and compared with a GC-MS method. Chromatographic analysis using a beta-cyclodextrin stationary phase was performed after active and passive air sampling by adsorption on activated charcoal and pressurized fluid extraction. The analytes were completely separated and quantified using both methods, although GC-MS provided better resolutions and lower detection limits than HPLC. The HPLC method was unsuccessfully applied to the determination of benzene in real samples because its sensitivity was too low. Both methods were applied to the analysis of certified reference materials and air samples collected in several workplaces. Statistical comparison showed that HPLC and GC-MS provided analogous accuracy.
