Other extraction techniques proposed for the determinationof 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 directSPME [14,15]. Sampling by HS-SPME is more suitable when matrixcould affect the determination of analytes [16,17]. The use ofHS-SPME for VOCs determination, especially for BTEX, is a goodalternative as extraction procedure for water samples [18–22].