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中国无机分析化学:2023,13(11):1264-1270
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直接进样-电感耦合等离子体发射光谱(ICP-OES)法测定六氟磷酸锂电解液中17种杂质元素
熊壮, 李鹰, 李剑
(杭州谱育科技发展有限公司)
Determination of 17 Impurity Elements in Lithium Hexafluorophosphate Electrolyte by Direct Injection Inductively Coupled Plasma optical Emission Spectrometry(ICP-OES)
Zhuang Xiong, Ying Li, Jian Li
(Hangzhou Puyu Technology Co. Ltd.,Hangzhou)
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投稿时间:2022-12-19    修订日期:2022-12-26
中文摘要: 电解液,被称为锂电池的血液,对锂离子电池的主要性能起着决定的作用。六氟磷酸锂(LiPF6)是生产电解液的核心材料,电解液中的杂质离子会对电池性能造成极大的负面影响。因此,掌握锂离子六氟磷酸锂电解液中杂质元素的检测方法显得格外重要。传统的消解后测试的方法会造成部分元素损失,会引入新的污染,对低含量的元素难以准确定量,标准推荐的稀释剂需要用到电子级碳酸甲乙酯,成本较高。本文采用30%(v/v)乙醇水溶液稀释六氟磷酸锂电解液后直接进样,搭配电感耦合等离子体发射光谱(ICP-OES)有机进样系统,采用标准曲线法,测定了六氟磷酸锂电解液中的铝、砷、钙、镉、钴、铬、铜、铁、汞、钾、镁、钼、镍、钠、铅、硫、锌共17种杂质元素含量。实验中对ICP-OES最佳工作条件(包括雾化室温度、雾化气流量、雾化器、蠕动泵转速、电源功率、氧气流量)进行了优化,结果表明雾化室温度在5℃,雾化气流量在0.6 L?min-1,使用的雾化器为OneNeb雾化器,蠕动泵转速为50转?min-1,电源功率为1150w,氧气流量为50 mL?min-1时,各元素的灵敏度、试液的消耗、耗材的磨损能达到最佳效果。结果表明17种分析元素标准曲线的线性相关系数(r)不小于0.999,方法检出限在0.0163 ~ 0.0940 mg/L之间,精密度小于3.41%,加标回收率在90.2% ~ 110%之间,不同稀释剂处理后的元素含量相对误差在5%以内,证明该方法是分析六氟磷酸锂电解液中杂质元素有效、简单且快捷的方法。
Abstract:Electrolyte, known as the blood of lithium battery, plays a decisive role in the main performance of lithium ion battery. Lithium hexafluorophosphate (LiPF6) is the core material for the production of electrolyte, and the impurity ions in the electrolyte will have a great negative impact on the battery performance. Therefore, it is particularly important to master the monitoring methods of impurity elements in lithium ion lithium hexafluorophosphate electrolyte. The traditional digestion before testing will cause some element loss and pollution, and it is difficult to accurately quantify the elements with low content. The standard recommended diluent needs to use electronic methyl ethyl carbonate, which is expensive. In this paper, the contents of 17 impurity elements in lithium hexafluorophosphate electrolyte, including Aluminum, Arsenic, Calcium, Cadmium, Cobalt, Chromium, Copper, Iron, Mercury, Potassium, Magnesium, Molybdenum, Nickel, Sodium, Lead, Sulfur and Zinc, were determined by standard curve method in a direct injection system coupled with inductively coupled plasma atomic emission spectrometry (ICP-OES), in which lithium hexafluorophosphate electrolyte was solution diluted by a 30% (v/v) ethanol aqueous. The best working conditions of ICP-OES (including the temperature of the atomizing chamber, the flow of atomizing gas, the atomizer, the rotational speed of the peristaltic pump, the power supply, and the oxygen flow) were optimized in the experiment. The results showed that when the temperature of the atomizing chamber was 5 ℃, the flow of atomizing gas was 0.6 L?min-1, the atomizer used was OneNeb atomizer, the rotational speed of the peristaltic pump was 50 rpm?min-1, the power supply was 1150w, and the oxygen flow was 50 mL?min-1, the sensitivity and the consumption of test solution and wear of consumables can achieve the best effect. The results showed that the linear correlation coefficient (r) of the standard curves of 17 analytical elements was not less than 0.999, the detection limit of the method was 0.0163~0.0940 mg/L, the precision was less than 3.41%, and the spiking recovery was 90.2%~110%, The relative error of element content of different diluents is within 5%, which proves the method is effective, simple and fast for the analysis of trace elements in lithium hexafluorophosphate electrolyte.
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基金项目:国家重点研发计划“基础科研条件与重大科学仪器设备研发”(2021YFF0700804)
引用文本:
熊壮,李鹰,李剑.直接进样-电感耦合等离子体发射光谱(ICP-OES)法测定六氟磷酸锂电解液中17种杂质元素[J].中国无机分析化学,2023,13(11):1264-1270.
Zhuang Xiong,Ying Li,Jian Li.Determination of 17 Impurity Elements in Lithium Hexafluorophosphate Electrolyte by Direct Injection Inductively Coupled Plasma optical Emission Spectrometry(ICP-OES)[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(11):1264-1270.

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