CAJ | 학술논문

建立了电感耦合等离子体质谱(ICP-MS)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 ICP-MS 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。
건립료전감우합등리자체질보(ICP-MS)법직접측정륙불린산리중26충잡질원소(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)적분석방법。양품용무수을순용해후직접용 ICP-MS 측정。통과재등리자체중인입양기,피면양품용액중고농도탄냉응침적재질보추접구화리자투경상도치분석원소령민도적강저적현상,채용팽당/반응지(CRC)기술교정료다원자리자질보간우,선택기체필배법교정료기본효응。결과표명,26충잡질원소정량표준곡선적선성상관계수불소우0.9995,검출한재0.6~31.9 ng/ L 지간,RSD 위2.5%~7.3%,가표회수솔재90.6%~108.6%지간。본방법능만족륙불린산리중잡질원소적분석요구。
An inductively coupled plasma mass spectrometry ( ICP-MS) 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 ICP-MS. 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.