Determination of volatile alkyl sulfides in wastewater by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry

J Chromatogr A. 2002 Jul 19;963(1-2):249-57. doi: 10.1016/s0021-9673(02)00543-5.


An analytical procedure based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to mass spectrometry in the electron impact mode has been developed for the determination of low-molecular-mass sulfides and disulfides in wastewater. Parameters affecting to the extraction of these volatile alkyl sulfides (VASs) with the SPME, such as the extraction temperature, sample volume, pH and the NaCl addition to the matrix, have been optimised using a polydimethylsiloxane-Carboxen fibre. The linear dynamic range was close to three orders of magnitude for all the studied compounds. Detection limits of 4 ng l(-1) for dimethyl sulfide, 0.7 ng l(-1) for ethylmethyl sulfide, 5 ng l(-1) for diethyl sulfide and 1 ng l(-1) for dimethyl disulfide were achieved, with a relative standard deviation between 4 and 6%. The developed analytical methodology was applied to determine those VASs in different wastewaters.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Hydrogen-Ion Concentration
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Sulfides / analysis*
  • Water Pollutants, Chemical / analysis*


  • Sulfides
  • Water Pollutants, Chemical