Spectral cathode copper standard samples were prepared in the intermediate frequency induction furnace by adding necessary additives into 5N-level cathode copper. The manufacturing process, including design of the component, selection of raw materials, characterization of homogeneity, analysis of standards, statistical treatment of data and confirmation of values and standards deviation are presented in this manuscript. The effects of the preparation technological parameters on the sample variance were studied and the optimal processing conditions were obtained as follows: the casting temperature is 1200°C, the stirring rate is 120 rpm, the stirring time is 1 min, the heat preservation period is 25 min and argon dosage is 0.4 m3/kg. The spectral standard sample for cathode copper obtained under these conditions has a preferred orientation on the (220) plane and has been approved as a national level standard sample (No. GSB 04-2707-2011) by China National Standard Sample Technical Committee due to its compact and uniform structure, good stability, high accuracy and reliability.