In the present work, results from a survey on mercury concentration in sediments and soils from a gold mining area along the Vila Nova river, in Amapá State, Brazil, are presented. These values were compared with those from the Igarapé Pedra Preta basin, an area unaffected by mining activities. Total mercury contents were determined in the muddy (silt+clay) fraction of the sediments and in the <2 mm fraction of the soils using radiochemical neutron activation analysis (RNAA). The detection limit of the method was 54 µg·kg–1 for soils and 14 µg·kg–1 for sediments when 200 mg of sample were analysed. The Hg results obtained from a comparison between our current method (RNAA) and CV AAS are also presented. Mercury levels showed to be very high in the soils and sediments collected in the Vila Nova river (up to 2 mg·kg–1) when compared to background values (0.3 mg·kg–1) for this region. An enrichment factor was calculated, using Al as a normalizing factor. It showed values up to 8 in sediments of the Vila Nova river basin, indicating a relatively high degree of pollution as compared to the values of about 1 for the samples of the Igarapé Pedra Pretra basin.