Three protocols (Method I: ion chromatography (IC) and extraction chromatography (EC), Method II: precipitation followed by IC, and Method III: adsorption onto MnO2 followed by IC-EC) were investigated to determine their applicability for the separation and pre-concentration of 226Ra in sediments. 226Ra recoveries, measured using the isotope dilution method with 228Ra as yield tracer, and the removal of spectral and non-spectral interferences were evaluated. The formation of polyatomic interferences at m/z = 226 from elements found in the matrix of sediments was also investigated to assess the level of separation required. Methods I and III were found to be the most effective with respect to recoveries and interference removal. The efficiency of a rapid microwave based protocol for the complete digestion of 1 g of sediment is also described. The method was tested and 226Ra concentrations in the millibecquerel range (fg) were determined in a standard reference material and sediment cores collected from Lake Baikal.