有机溶剂溶样电感耦合等离子体质谱法直接测定六氟磷酸锂中26种杂质元素

刘宏伟等
摘 要 建立了电感耦合等离子体质谱(ICPMS)法直接测定六氟磷酸锂中26种杂质元素(Be, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Sr, Zr, Mo, Pd, Ag, Cd, Sn, Sb, Ba, Pb)的分析方法。样品用无水乙醇溶解后直接用ICPMS测定。通过在等离子体中引入氧气,避免样品溶液中高浓度碳冷凝沉积在质谱锥接口和离子透镜上导致分析元素灵敏度的降低的现象,采用碰撞/反应池(CRC)技术校正了多原子离子质谱干扰,选择基体匹配法校正了基本效应。结果表明,26种杂质元素定量标准曲线的线性相关系数不小于0.9995,检出限在0.6~31.9 ng/L之间,RSD为2.5%~7.3%,加标回收率在90.6%~108.6%之间。本方法能满足六氟磷酸锂中杂质元素的分析要求。
关键词 电感耦合等离子体质谱法; 六氟磷酸锂; 无水乙醇; 碰撞/反应池; 杂质元素
1 引 言
锂离子电池电解质在电池中起着正负极之间电荷传输的作用,是影响电池工作温度、比能量、循环效率以及安全性能的关键原材料之一,主要由电解质锂盐、混合有机溶剂和添加剂组成。由于锂离子电池的电压较高且电池负极材料较为活泼,需采用非水电解质。非水电解质六氟磷酸锂(LiPF6)在有机碳酸酯类溶剂中具有溶解度较大、电导率高、电化学稳定性好等特点,是锂电池电解质的重要组成部分[1],其杂质元素严重影响锂离子电池的电化学性能。
目前,LiPF6中杂质元素的分析主要采用电感耦合等离子体发射光谱
3 结果与讨论
3.1 仪器信号的稳定性
LiPF6样品中杂质元素含量低,有机质含量很高,采用无水乙醇稀释, 进一步加大了有机质的浓度,在实验过程中会造成炬管、锥口和离子透镜上积碳,影响分析信号的稳定性。本实验采用附加的质量流速控制器将氧气加入至等离子体中,通过向辅助气流中混入氧气,使高碳有机物与氧气燃烧,以消除碳冷凝沉积在接口和离子透镜上。考察了氩气中氧气混入量分别为References
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Direct Determination of Impurity Elements in High Purity
Lithium Hexafluorophosphate Dissolved with Ethyl Alcohol
by Inductively Coupled Plasma Mass Spectrometry
LIU HongWei*, ZHANG Ping, HU HanXiang
(College of Material and Chemical Engineering, Hunan Institute of Technology, Hengyang 421002, China)
Abstract An inductively coupled plasma mass spectrometry (ICPMS) was developed for the direct determination of Be, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Zr, Mo, Sr, Cd, Ba, Pd, Ag, Sn, Au and Pb in lithium hexafluorophosphate. The sample was dissolved with absolute ethyl alcohol to analyze the above 26 impurity elements in the solution by ICPMS. The condensation and deposition of high concentrations of carbon in mass cone interface and ion lens, which will decrease the sensitivity of element analysis, can be avoided effectively by introducing O2 to plasma. The mass spectral interferences of polyatomic ions to analytes were corrected by collision reaction cell (CRC). The matrix matching method was used to corrected matrix effect. Satisfactory linearity of each working curve of 26 impurity elements was obtained. The correlation coefficients being over 0.9995, the detection limits for the investigated elements were in the range of 0.6-32 ng/L, the relative standard deviation of each element within 2.5%-7.3%, and the recovery of each element at 90.6%-108.6%. The method had been applied to the determination of trace elements in lithium hexafluorophosphate with satisfactory results.
Keywords Inductively coupled plasma mass spectrometry; Lithium hexafluorophosphate; Absolute ethyl alcohol; Collision reaction cell; Impurity elements
(Received 18 February 2014; accepted 23 March 2014)
by Inductively Coupled Plasma Mass Spectrometry
LIU HongWei*, ZHANG Ping, HU HanXiang
(College of Material and Chemical Engineering, Hunan Institute of Technology, Hengyang 421002, China)
Abstract An inductively coupled plasma mass spectrometry (ICPMS) was developed for the direct determination of Be, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Zr, Mo, Sr, Cd, Ba, Pd, Ag, Sn, Au and Pb in lithium hexafluorophosphate. The sample was dissolved with absolute ethyl alcohol to analyze the above 26 impurity elements in the solution by ICPMS. The condensation and deposition of high concentrations of carbon in mass cone interface and ion lens, which will decrease the sensitivity of element analysis, can be avoided effectively by introducing O2 to plasma. The mass spectral interferences of polyatomic ions to analytes were corrected by collision reaction cell (CRC). The matrix matching method was used to corrected matrix effect. Satisfactory linearity of each working curve of 26 impurity elements was obtained. The correlation coefficients being over 0.9995, the detection limits for the investigated elements were in the range of 0.6-32 ng/L, the relative standard deviation of each element within 2.5%-7.3%, and the recovery of each element at 90.6%-108.6%. The method had been applied to the determination of trace elements in lithium hexafluorophosphate with satisfactory results.
Keywords Inductively coupled plasma mass spectrometry; Lithium hexafluorophosphate; Absolute ethyl alcohol; Collision reaction cell; Impurity elements
(Received 18 February 2014; accepted 23 March 2014)
by Inductively Coupled Plasma Mass Spectrometry
LIU HongWei*, ZHANG Ping, HU HanXiang
(College of Material and Chemical Engineering, Hunan Institute of Technology, Hengyang 421002, China)
Abstract An inductively coupled plasma mass spectrometry (ICPMS) was developed for the direct determination of Be, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Zr, Mo, Sr, Cd, Ba, Pd, Ag, Sn, Au and Pb in lithium hexafluorophosphate. The sample was dissolved with absolute ethyl alcohol to analyze the above 26 impurity elements in the solution by ICPMS. The condensation and deposition of high concentrations of carbon in mass cone interface and ion lens, which will decrease the sensitivity of element analysis, can be avoided effectively by introducing O2 to plasma. The mass spectral interferences of polyatomic ions to analytes were corrected by collision reaction cell (CRC). The matrix matching method was used to corrected matrix effect. Satisfactory linearity of each working curve of 26 impurity elements was obtained. The correlation coefficients being over 0.9995, the detection limits for the investigated elements were in the range of 0.6-32 ng/L, the relative standard deviation of each element within 2.5%-7.3%, and the recovery of each element at 90.6%-108.6%. The method had been applied to the determination of trace elements in lithium hexafluorophosphate with satisfactory results.
Keywords Inductively coupled plasma mass spectrometry; Lithium hexafluorophosphate; Absolute ethyl alcohol; Collision reaction cell; Impurity elements
(Received 18 February 2014; accepted 23 March 2014)
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