This study proposes a simple and innovative synthesis route for a goethite-calcite nanocomposite. This synthesis is summarised by three sequential precipitation reactions: (1) precipitation of nanosized acicular goethite (alpha-FeOOH) using a high OH/Fe molar ratio (=5); (2) instantaneous precipitation of portlandite (Ca(OH)(2)) by adding CaCl2 salt to a goethite alkaline suspension (2NaOH + CaCl2 -> Ca(OH)(2) + 2NaCI) and; (3) sub-micrometric calcite precipitation by injection of CO2 into a goethite-portlandite alkaline suspension (Ca(OH)(2) + CO2 -> CaCO3 + H2O). The XRD patterns have confirmed the goethite and calcite mineral composition in the composite precipitated at 30 and 70 degrees C. FESEM and TEM observations have revealed the formation of nanosized goethite particles well dispersed with sub-micrometric calcite particles, leading to an orange-brown colour nanocomposite with high specific surface area of around 92 m(2)/g for a composite synthesized at 30 degrees C and 45 m(2)/g for a composite synthesized at 70 degrees C. Both values were determined using the conventional BET method on N-2 sorption isotherms. Finally, a goethite/calcite weight ratio equal to 0.8 in the composite was determined by Thermogravimetric Analysis (TGA). Additionally, some adsorption experiments carried out at two different pH values revealed that the goethitecalcite composite has a good sequestration capacity for Cu > Cd > As(III) > Se(IV) > As(V). Conversely, the Se(VI) did not show any chemical affinity with the goethite-calcite composite under the physico-chemical conditions studied. In practice, the goethite-calcite composite can neutralise acidic wastewater by slight calcite dissolution, enhancing the removal of heavy metals (e.g. Cu and Cd) at the calcite-solution interfaces. (C) 2012 Elsevier B.V. All rights reserved.