Advances in the graphitization protocol at the Radiocarbon Laboratory of the Universidade Federal Fluminense (LAC-UFF) in Brazil

In this paper, we summarize the sample preparation methods currently used at the Radiocarbon Laboratory of the Universidade Federal Fluminense (LAC-UFF) in Brazil. We also report on a series of results with regards to the graphitization protocol. Tests with different temperatures and baking times were performed, and carbon stable isotope ratios of graphite were measured by an EA–IRMS (elemental analyzer coupled with an isotopic ratio mass spectrometer) to infer the completeness of the graphitization reaction. We monitored the muffle furnace temperature using an independent thermocouple and found a −60°C offset, which may have caused the lower graphitization yields (detected from the large isotopic fractionation on several reference materials targets). At a temperature of 520°C, the isotopic fractionation in the graphitization reaction was systematically lower (−5‰ in average) and the overall scattering was reduced. As long as isotopic fractionation corrections are made using the online stable isotopes ratios provided by the AMS system, the accuracy of the 14C results should be maintained.