Lake Três Irmãs (LTI), the largest upland lake in the Brazilian Amazonia, located in Serra dos Caraj as, was characterized using multi-elemental and isotope geochemistry (d 13 C and d 15 N) to understand the significance of organic and inorganic sources, weathering and sedimentary processes on the distribution of elements in lake bottom (surficial) sediments. Carbon and nitrogen isotopes from sedimentary organic matter suggest C3 terrestrial plants (forests > canga vegetation), macrophytes and freshwater DOC as the main sources. Sediments are depleted in most of the major oxides (except Fe 2 O 3 and P 2 O 5) when compared to upper continental crust (UCC) and their spatial distribution is highly influenced by catchment lithology. Principal Component Analysis revealed that most of the trace elements (Ba,