电感耦合等离子体发射光谱法测定普鲁士蓝类正极材料中铁和钠
张开砚
三峡大学分析测试中心,湖北宜昌 443002
Determination of Fe and Na in Prussian blue cathode materials by inductively coupled plasma emission spectrometer
ZHANG Kaiyan
Analysis and testing center, CTGU.Yichang 443002, China
摘要:采用电感耦合等离子体发射光谱法同时测定钠离子电池普鲁士蓝类正极材料中铁、钠元素的含量。分别对称样质量、样品消解用酸的种类和用量进行了研究,结果表明20 mg普鲁士蓝类正极材料加入15 mL浓盐酸,加热保温约1 h,可完全消解。目标物的分析谱线为Fe 238.204 nm,Na 589.592 nm。仪器最佳工作参数:发射功率为1.2 kW,雾化器流量为0.6 L/min,观测方向为轴向。综合采用基体匹配法和多谱线拟合校正方法消除干扰。按照该方法测定,铁、钠标准曲线的线性相关系数均大于0.999,检出限小于0.05μg/mL。样品加标回收率为100.7%~102.3%。对同一样品处理6次,测定值的相对标准偏差为0.817%~1.980%。
Abstract:The contents of Fe and Na in the Prussian blue cathode material were determined simultaneously by inductively coupled plasma emission spectrometry. The sample weighing, the type and amount of acid were studied respectively. The results showed that 20 mg Prussian blue cathode material with 15 mL of concentrated hydrochloric acid could be completely digested by heating and holding for about 1 h. The analytical lines of the target were Fe 238.204 nm and Na 589.592 nm. The best working parameters of the instrument were 1.2 kW of the emission power, 0.6 L/min of the flow rate and axial of the observation direction. At the same time, the matrix matching method and the multi-spectral line fitting correction method (MSF) were used to eliminate the interference. Under the optimal working conditions, the linear correlation coefficient of the standard curve was more than 0.999, and the detection limit was less than 0.05μg/mL. The recovery rate of sample standard addition was 100.7%-102.3%. The same sample was processed 6 times, and the relative standard deviations of the test results were 0.817%-1.980%.
关键词:普鲁士蓝类正极材料;电感耦合等离子体发射光谱法;钠离子电池;铁;钠
Keywords:Prussian blue cathode material; inductively coupled plasma emission spectrometer; sodium ion battery;Fe; Na
本文引用格式:
张开砚.电感耦合等离子体发射光谱法测定普鲁士蓝类正极材料中铁和钠[J].化学分析计量,2022,31(8):26.
ZHANG Kaiyan. Determination of Fe and Na in Prussian blue cathode materials by inductively coupled plasma emission spectrometer[J]. Chemical Analysis and Meterage,2022,31(8):26.
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