High‐grade periodate is relatively expensive, but is required for many sensitive applications such as the synthesis of active pharmaceutical ingredients. These high costs originate from using lead dioxide anodes in contemporary electrochemical methods and from expensive starting materials. A direct and cost‐efficient electrochemical synthesis of periodate from iodide, which is less costly and relies on a readily available starting material, is reported. The oxidation is conducted at boron‐doped diamond anodes, which are durable, metal‐free, and nontoxic. The avoidance of lead dioxide ultimately lowers the cost of purification and quality assurance. The electrolytic process was optimized by statistical methods and was scaled up in an electrolysis flow cell that enhanced the space–time yields by a cyclization protocol. An LC‐PDA analytical protocol was established enabling simple quantification of iodide, iodate, and periodate simultaneously with remarkable precision. The electrochemical synthesis of periodate from iodide at boron‐doped diamond (BDD) anodes was developed, which in contrast to lead dioxide anodes are sustainable and durable. Toxic contaminations are hereby prevented, ultimately reducing the cost of purification. This opens the door for the broad application of periodate for demanding applications, such as the synthesis of active pharmaceutical ingredients.