A novel approach to process carbonate samples for radiocarbon measurements with helium carrier gas

Most laboratories prepare carbonates samples for radiocarbon analysis by acid decomposition in evacuated glass tubes and subsequent reduction of the evolved CO2 to graphite in self-made reduction manifolds. This process is time consuming and labor intensive. In this work, we have tested a new approach for the preparation of carbonate samples, where any high-vacuum system is avoided and helium is used as a carrier gas. The liberation of CO2 from carbonates with phosphoric acid is performed in a similar way as it is often done in stable isotope ratio mass spectrometry where CO2 is released with acid in septum sealed tube under helium atmosphere. The formed CO2 is later flushed in a helium flow by means of a double-walled needle mounted from the tubes to the zeolite trap of the automated graphitization equipment (AGE). It essentially replaces the elemental analyzer normally used for the combustion of organic samples. The process can be fully automated from sampling the released CO2 in the septum-sealed tubes with a commercially available auto-sampler to the graphitization with the automated graphitization. The new method yields in low sample blanks of about 50000 years. Results of processed reference materials (IAEA-C2, FIRI-C) are in agreement with their consensus values.