As a required sample preparation method for 14C graphite, the Zn-Fe reduction method has been widely used in various laboratories. However, there is still insufficient research to improve the efficiency of graphite synthesis, reduce modern carbon contamination, and test other condition methodologies at Guangxi Normal University (GXNU). In this work, the experimental parameters, such as the reduction temperature, reaction time, reagent dose, Fe powder pretreatment, and other factors, in the Zn-Fe flame sealing reduction method for 14C graphite samples were explored and determined. The background induced by the sample preparation process was (2.06 ± 0.55) × 10–15, while the 12C– beam current were better than 40μA. The results provide essential instructions for preparing 14C graphite of ∼1 mg at the GXNU lab and technical support for the development of 14C dating and tracing, contributing to biology and environmental science.