The goal of this study was to omit the hazardous hydrofluoric acid for silica removal before fusion of barite-concrete. Furthermore, the goal was to establish a chemical separation technique to simultaneously determine the activity concentrations of 241 Am, 238 Pu, 239+240 Pu and 90 Sr of one sub-sample. After the fusion process, using Li-metaborate/Li-tetraborate, the colloidal silica could be successfully flocculated using polyethylene glycol (PEG-2000). A chemical separation scheme using the resins DGA-BIO-RAD AG 1-X2/UTEVA-DGA and TEVA for the actinides and DGA and Sr resin for Sr was successfully established, underlined by the quantitative 243 Am, 242 Pu and 85 Sr average tracer recoveries of at least 60%, and in best cases up to 86%.