摘要
探讨了电感耦合等离子体质谱(ICP-MS)法测定钴酸锂中Na、Mg、Al、K、Ca、Ti、Cr、Mn、Fe、Ni、Cu、Zn、As、Pd、Ag、Cd、Sn、Au、Pb、Bi等20种杂质元素的分析方法。样品用硝酸+盐酸经微波消解,试液用超纯水稀释后直接用ICP-MS法同时测定上述杂质元素。通过向八极杆碰撞/反应池(ORS)中引入氦气或氢气,消除高盐基体可能带来的多原子离子对待测元素的质谱干扰,选用45Sc、89 Y、103 Rh、205 Tl内标混合液校正基体干扰和漂移。20种待测元素的检出限在0.006～0.41μg/L之间。对锂离子电池正极材料钴酸锂样品进行精密度和准确度考察,相对标准偏差为1.3%～5.7%,加标回收率为91%～107%。采用实验方法对不同批号的钴酸锂样品进行测定,结果同其他方法(AAS,AFS,ICP-AES)测定值一致。
The analysis method of 20 impurity elements（Na,Mg,Al,K,Ca,Ti,Cr,Mn,Fe,Ni,Cu,Zn,As,Pd,Ag,Cd,Sn,Au,Pb and Bi）in lithium cobalt oxide by inductively coupled plasma mass spectrometry（ICP-MS）was discussed.The sample was dissolved via microwave digestion with nitric acid and hydrochloric acid.The sample solution was diluted with ultrapure water and then the impurity elements were directly determined by ICP-MS.Helium or hydrogen was introduced into octopole reaction system（ORS）to eliminate the mass interference of polyatomic ions from high salt matrix on testing elements.Mixed internal standard solution of 45Sc,89 Y,103 Rh and 205 Tl was selected to correct matrix interference and drifting.The detection limits of 20testing elements were between 0.006and 0.41μg/L.Precision and accuracy test were conducted on lithium-ion battery anode material（lithium cobalt oxide）samples.The relative standard deviations（RSD）were in the range of 1.3%5.7%.The recoveries of standard addition were 91%-107%.The proposed method was used to determine lithium cobalt oxide samples of different batches,and the results were consistent with those obtained by other methods（AAS,AFS and ICP-AES）.
出处
《冶金分析》
CAS
CSCD
北大核心
2013年第7期30-34,共5页
Metallurgical Analysis
基金
湖南省自然科学基金(12JJ6010
13JJ3123)
湖南省重点学科建设项目资助
关键词
电感耦合等离子体质谱法
钴酸锂
八极杆碰撞
反应池
杂质元素
inductively coupled plasma mass spectrometry
lithium cobalt oxide
octopole reaction system（ORS）
impurity elements
