New approach on the alkylthiol determination in water byin situderivatization SPME followed by GC-ECD/NPD analysis

Autor: Maria Llompart, Roberto Alzaga, Josep M. Bayona, Carmen Garcia-Jares, Carmen Salgado-Petinal
Rok vydání: 2005
Předmět:
Zdroj: International Journal of Environmental Analytical Chemistry. 85:543-552
ISSN: 1029-0397
0306-7319
DOI: 10.1080/03067310500107195
Popis: Alkylthiols are very reactive and highly volatile compounds, and thus it is difficult to determine these in the water phase. In the present work, an in situ derivatization step prior to solid-phase microextraction (SPME) has been developed for their determination in water samples. The dinitrobenzylation reaction was selected because the high chemical stability of the corresponding thioethers formed provides a significant increase in the distribution coefficient between the SPME fibre and the aqueous phase, and a potential increase in the selectivity and sensitivity. Therefore, different derivatization reaction conditions (i.e. pH, temperature, reaction time and derivatizating reagent concentration) have been studied. Then, the main parameters affecting to the SPME process, that is coating selection, extraction time profile, extraction and desorption temperatures, have been optimized. Finally, a method based on a simple 2,4-dinitrophenylation reaction at pH 8–10, in 60 min at 75°C, coupled to direct SPME u...
Databáze: OpenAIRE