A perfluorooctane sulfonic acid (PFOS) biomonitoring survey was conducted on great tit (Parus major) and blue tit (Parus caeruleus) nestlings from Blokkersdijk, a bird reserve in the proximity of a fluorochemical plant in Antwerp (Belgium) and Fort IV, a control area. PFOS, together with 11 organochlorine pesticides, 20 polychlorinated biphenyl congeners and 7 polybrominated diphenyl ethers were measured in liver tissue. The hepatic PFOS concentrations at Blokkersdijk (86-2788 and 317-3322 ng/g wet weight (ww) for great and blue tit, respectively) were among the highest ever measured and were significantly higher than at the control area (17-206 and 69-514 ng/g ww for great and blue tit, respectively). The hepatic PFOS concentration was species- and sex-independent and correlated significantly and positively with the serum alanine aminotransferase activity and negatively with the serum cholesterol and triglyceride levels in both species but did not correlate with condition or serum protein concentration. In the great tit, a significant positive correlation was observed between the liver PFOS concentration and the relative liver weight. In the blue tit, the hepatic PFOS concentration correlated positively and significantly with hematocrite values. None of the investigated organohalogen pollutants except for PFOS were suggested to be involved in the observed biological alterations.