离子色谱法测定锂离子电池正极原材料中阴离子杂质  

Determination of anion components in raw materials for positive electrode of lithium-ion batteries by ion chromatography

作　　者：郑秀瑾 张苗苗 王永文 宁鹏 尹登刚 ZHENG Xiujin;ZHANG Miaomiao;WANG Yongwen;NING Peng;YIN Denggang(Qingdao Shenghan Chromatogram Technology Co.,Ltd.,Qingdao 266101)

机构地区：[1]青岛盛瀚色谱技术有限公司,青岛266101

出　　处：《分析试验室》2020年第11期1345-1350,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立了锂离子电池正极原材料(LiOH,Li2CO3,Ni(OH)2,Ni2CO3)中F-,Cl-,NO3-,SO24-的离子色谱分析法。100 mg样品加800μL磷酸溶液(V:V,1:1)助溶,超纯水溶解,超声提取后,过H柱和0. 22μm滤膜后,选用SH-AP-1色谱柱进行色谱分离,18. 0~40. 0mmol/L KOH淋洗液进行梯度洗脱,采用电导检测器检测,外标法定量。结果表明,4种阴离子的峰面积与其质量浓度在一定范围内呈良好线性关系,检出限(S/N=3)在0. 244~3. 04μg/L之间。以NiCO3样品为基体进行加标回收实验,回收率在90. 0%~108. 6%之间,相对标准偏差(n=6)在0. 1%~2. 1%之间。该方法可用于锂离子电池正极原材料中杂质阴离子的检测。A ion chromatography method was developed to detect F-,Cl-,NO3-and SO24-in raw materials( lithium hydroxide,lithium carbonate,nickel hydroxide,nickel carbonate) for positive electrode of lithium-ion batteries. 100 mg sample was dissolved with 800 μL phosphoric acid solution( V: V,1: 1) and ultrapure water,extracted ultrasonically,filtrated with H column and 0. 22 μm membrane. SH-AP-1 was selected as the separation column,18. 0-40. 0 mmol/L KOH solutions were used as the mobile phase in gradient elution. The constituents of sample were analyzed by a conductivity detector,and quantified by external standard method. The methoud showed that the peak areas of the anion components presented a good linear relationship in definite range of mass concentration. LODs( S/N = 3) were in the range of 0. 244-3. 04 μg/L. On the base of nickel carbonate sample,the recoveries were in the range of 90. 0%-108. 6%,with RSDs( n = 6) of 0. 1%-2. 1%.The method could be used for determination of the anion components in raw materials for positive electrode of lithium-ion batteries.

关 键 词：离子色谱法 锂离子电池 正极原材料 碳酸镍 

分 类 号：O657.7[理学—分析化学] TM912[理学—化学]