Chromatografic separation of Co(Ⅱ) & Ni(Ⅱ) with CL P507 Levextrel resin was studied. The method of adding ligand glycine in feed was developed instead of resin transformation. The effects of eluent's pH value,amounts and ratio of Co,Ni on separation were examined. Samples containing 1600μg metals with Co/Ni ratio of 1～100 can be separatedeffectively by 5g resin at pH=3.40. The actions of glycine ascoordination and buffer on separation process were investigated.