Abstract: K4648 nickel-based superalloy control samples were prepared by vacuum induction melting and investment casting. To improve the quality of control samples, a smelting process combining high-temperature refining and low-temperature mold filling and a gating system with sequential solidification were adopted, and a stepwise homogenization heat treatment process was applied. X-ray flaw detection, microstructure observation, energy spectrum analysis and uniformity inspection of alloy elements were carried out for the control sample blanks. The results show that the prepared K4648 cast nickel-based superalloy samples has complete and dense structure, fine microstructure and uniform distribution of alloy elements, meeting the usage requirements of control samples. Moreover, the quality control process is simple and can be used for preparing control samples of other grades of cast nickel-based superalloys, fulfilling the needs for chemical composition detection of cast nickel-based superalloys by using spark discharge atomic emission spectrometry.