Abstract:Abstract: The content of nickel in crude copper was determined by Na2EDTA back titration. Sodium citrate, sodium thiosulfate and tartaric acid were used as hiding agents. Dimethylglyoxime was precipitated and separated .Xylenol orange was used as indicator and excessive Na2EDTA was added to back titration with zinc chloride standard solution .The interference of copper and other impurities can be separated by this method .The relative standard deviation(RSD, n=9) of the test results is 0.0456%-0.2409% and the recovery rate 99.73%-100.30% . If there is residue, the residue will be digested after filtrating, and the content of nickel in the insoluble residue will be determined by spectrum .It can meet the test requirement of daily samples.