The nickel has been separated and precipitated with dimethylglyoxime in the usual manner and dissolved the precipitates with hydrochloric acid. To the nickel solution, 0.2g of Murexide as an indicator and 5 ml of 20 percent tri-ethanol amine solution were added and titrated with a standard solution of EDTA. At the end point the color changes from yellow to deep purple. In this paper, the purpose is that conditions for titration and for separation from the interfering substances were investigated and a suitable procedure was found and applied on the determination of nickel in Korean nickel ores.