Abstract Accurate analysis of coexisting calcite and dolomite for d13C and d18O is generally hindered by the difficulty in the physical separation of these minerals. The difference in the reaction rates of calcite and dolomite with phosphoric acid, has been used to chemically separate these carbonates. Previously established procedures are only suitable for samples containing 1:1 calcite-dolomite pairs. However, these are sometimes tedious and time-consuming. Using mixtures of calcite and dolomite, two different selective acid extraction procedures (for reactions at 25°C), one for calcite-rich and the other for dolomite-rich carbonates, have been developed. Reduction of grain size (to 37μm - 45μm) increased the reaction rate and hence decreased the total reaction time to a reasonable interval (=72 hours for dolomite). Applying these procedures, d13C and d18O of calcite and dolomite/ankerite of carbonatites from Amba Dongar and Sung Valley carbonatite complexes of India were measured and their temperatures of crystallization determined. Accurate isotopic compositions of individual carbonates of calcite-dolomite mixtures can be determined for geological interpretations by these procedures.