Sixty-four wastewater samples were collected from three different geographical areas (estuarine of Jucar, Cullera and Santa Pola)located at the Comunidad Valenciana (Spain). Sampling campaigns were carried out every three months corresponding to the seasonal period (February (winter), April (spring), July (summer) and October (autumn)). Samples were collected in pre-cleaned amber glass bottles (1 L). Sampling bottles were completely filled to avoid VOCs migration from the aqueous solution to the headspace. Two 10-mL fractions of each sample were placed in the 22 mL glass vials immediately after their arrival to the laboratory. HS sampling and GC analysis were carried out in each of these vials.