Abstract：Nickel-cobalt-manganese composite hydroxide is the main raw material for the preparation of lithium-ion battery anode material, i.e., LiNiCoMnO2. The content of Ni is an important index for quality control. If Ni content in nickel-cobalt-manganese composite hydroxide was directly analyzed by EDTA titration, the coexisting Co and Mn would cause interference with the determination results.The nickel-cobalt-manganese composite hydroxide sample was dissolved with hydrochloric acid firstly. Then dimethylglyoxime was added as precipitant in a slightly ammoniacal solution. Ni2+ could react with dimethylglyoxime to form red precipitate, realizing the separation of Ni2+ from Co2+ and Mn2+. The precipitate was dissolved and the content of Ni2+ was determined by EDTA titration. Consequently, a determination method of Ni in nickel-cobalt-manganese composite hydroxide by EDTA titration after precipitation separation using dimethylglyoxime was established. The experimental conditions were optimized: the dosage of precipitant was 1.9 times of theoretical value; the initial pH for precipitation was 8-9; the aging time was 30min; the aging temperature was 80℃; the precipitate was washed for 6 times. The determination results of simulation sample solution indicated that the interference caused by trace impurity elements in sample (such as Mg, Fe, Cu, Zn, Cr and Cd) could be ignored. The accuracy tests of Ni were conducted using nickel-cobalt-manganese composite hydroxide samples including NCM111 type, NCM622 type and NCM811 type. The relative standard deviations (RSD, n=11) of determination results were between 0.29% and 0.48%. The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) combined with EDTA titration. The recoveries of NCM523 type and NCM811 type nickel-cobalt-manganese composite hydroxide were between 96.9% and 102.5%.
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FU Hai-kuo, HE Hai-mei. Determination of nickel in nickel-cobalt-manganese composite hydroxide by EDTA titration after precipitation separation using dimethylglyoxime. , 2020, 40(7): 47-51.
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