The invention discloses a process for separating an electrode for a membrane-electrode assembly of a fuel cell and apparatus therefore. In particular, during the electrode separating process, only an electrode is separted from the decal transfer film on which the electrode is coated, without any damage, by a freezing method for freezing the specimen on the deionized water surface, and thus, wasting the experience MEA is prevented. Thus, mechanical properties of the pristine electrode can be rapidly quantified in advance, and therefore, long term durability evaluation period during developing MEA having excellent durability is substantially reduced.