Many metal radioisotopes (RIs) are produced using cyclotrons, followed by purification and processing for further use. Because some metal RIs have short half-lives (~10 h), rapid, effective separation and purification methods are recommended. Recently, electrochemical separation was utilized to separate Cu from Ni target by selective deposition. Additionally, a universal separation method via selective chelate formation was used to separate Ga from Zn target under milder acidic conditions than those required for conventional RI separation methods. Electrodialytic ion transfer has also been successfully used for matrix conversion and enrichment. These fast methods for separating short-half-life RIs are highly efficient. In this chapter, the methods and practical approaches for separating metal RIs are discussed in detail.