The Spring and Autumn and Warring States Periods were an important stage in the development of metal smelting and casting techniques in China; the main decorative crafts of this period included gold and silver inlaying. In recent years, a number of important Xirong remains have been discovered in Gansu, with the Shijia and Yucun site in Ningxian County and the Majiayuan site in Zhangjiachuan Hui Autonomous County as representatives. The metallic relics unearthed at these sites provide us with precious physical evidence, which can more objectively reflect the craftsmanship standard of this historical stage. In our work, we took “S”-shaped gold, silver and iron ornaments unearthed at the Shijia cemetery and the Majiayuan site as the study objects, and used modern analytical techniques such as super depth-of-field microscopy, X-ray fluorescence spectrometry, and scanning electron microscopy, in combination with the artifacts unearthed at related Qin tombs, to conduct an in-depth exploration and discussion. Through the analysis of two “S”-shaped gold, silver and iron ornaments, it was found that the “amalgamated mercury” technique was adopted in the production process, and that the ornaments were finely polished after engraving. This discovery not only reveals the techniques for gold, silver and iron ornament production in this period, but also provides important historical reference for subsequent research, which further enriches the understanding of the material culture of gold, silver and iron ornaments and the development of its production process.