The aim of this study is to develop analytical methodologies for the assessment of total arsenic (As) and inorganic As species, fluoride, iron and manganese in groundwater samples used for human consumption in Uruguay, and to evaluate the possible correlations between them. For this, 50 samples of groundwater from north Uruguay were analyzed. The concentration ranges found were: tAs (0.94–58.9) μg L–1, F− (0.168–1.528) mg L−1, Fe (2.1–95.5) μg L–1, and Mn (0.12–138.6) μg L–1. More than half of the samples presented tAs concentration above WHO As limits for drinking water, with the corresponding risks for public health. Pearson correlations between tAs and F−, Fe and Mn were studied, resulting in strong positive correlations for As/F− and As/Fe. Preliminary results showed higher As(III) levels in the samples, which is in agreement with the reducing conditions of the aquifers.