The determination method of nickel content in LiCoxNiyMn1-x-yO2(0x,0y,x+y1)by using dimethylglyoxime precipitate separation-disodium ethylenediaminetetraacetate dihydrate titration was studied,the optimum operating conditions for precise and rapid determination of nickel content were:adding 30 ml 15% tartaric acid solution and 20 ml 50% ammonium acetate solution,the pH value was 6.5 when nickel was precipitating and the aging time was 0 min.The potentiometric method was used for determining manganese content precisely and rapidly.The EDTA titration method was also put forward to determine the total content of nickel,cobalt and manganese by using xylenol orange as indicator and hexamethylenetetramine(pH=6.0~6.2)as buffer mediator and under 100 ℃.The content of cobalt was calculated indirectly after aforementioned determination.The RSD of this method was below 0.71%,the recovery rate was between 97.40%~101.60% and the time was less than 60 min,the precise and rapid determination of nickel,cobalt and manganese content in LiCoxNiyMn1-x-yO2 was realized.