Other extraction techniques proposed for the determination of these compounds in water samples are static headspace (HS)coupled to solid-phase microextraction (SPME) [12], dynamic-headspace coupled to liquid-phase microextraction [13] and direct SPME [14,15]. Sampling by HS-SPME is more suitable when matrix could affect the determination of analytes [16,17]. The use of HS-SPME for VOCs determination, especially for BTEX, is a good alternative as extraction procedure for water samples [18–22].