真空辅助挥发-便携式气相色谱-质谱现场快速测定锂电池微漏  

Rapid On-site Detection of Microleakage of Lithium Battery Electrolytes by Vacuum-Assisted Volatilization-Portable Gas Chromatography-Mass Spectrometry

作　　者：陆欣鑫 张硕 徐恺 仇俊炜 朱惠君 陈雨琳 李晓旭[1] LU Xin-xin;ZHANG Shuo;XU Kai;QIU Jun-wei;ZHU Hui-jun;CHEN Yu-lin;LI Xiao-xu(School of Mechanical and Electrical Engineering,Soochow University,Suzhou 215021,China)

机构地区：[1]苏州大学机电工程学院,江苏苏州215021

出　　处：《质谱学报》2025年第2期149-159,I0002,共12页Journal of Chinese Mass Spectrometry Society

摘　　要：本工作开发了真空辅助挥发装置,基于吸附/热脱附-气相色谱-质谱(ATD-GC-MS)联用技术建立了一种针对锂电池电解液微量泄漏的现场快速检测方法。在采样体积300 mL、色谱进样分流比50:1、热脱附温度180℃的实验条件下,电解液中3种挥发性有机物的检出限和定量限分别为1.57~2.27μg/m^(3)和4.99~7.23μg/m^(3),且分别在7.85~5270μg/m^(3)和5078~89167μg/m^(3)浓度范围内呈现良好的线性关系,拟合优度系数(R2)大于0.997,加标回收率在84.21%~103.21%之间。当真空辅助挥发装置的压力设置为−27 kPa时,单次检测时间小于8 min。为进一步验证方法的实用性,设计了电解液微漏模拟装置,并对18650和21700圆柱型锂电池进行微漏检测实验。本方法操作简单、快速高效、测量精度高,适用于锂电池微量泄漏的现场快速检测。With the surge in demand for lithium-ion batteries in various fields,concerns about their safety have increased.Electrolyte leakage,as a critical safety hazard,often goes unnoticed due to its subtle occurrence and the volatility of electrolyte components.In the application of on-site analysis,gas sensors are limited by their sensitivity and qualitative capability.Traditional gas chromatographymass spectrometry(GC-MS)is not suitable for on-site analysis due to its size and inconvenient operation.Portable chromatography-mass spectrometer has the advantages of high efficiency,small size,light weight,and low power consumption,and is suitable for on-site determination of volatile organic compounds(VOCs).In this study,a vacuum-assisted volatilization system was developed,and a rapid on-site analytical method for microleakage of lithium battery electrolyte was established based on adsorption/thermal desorption-portable gas chromatography-mass spectrometry(ATD-GCMS).Under the experimental conditions of a sampling volume of 300 mL,a split ratio of 50:1 and a thermal desorption temperature of 180℃,the limit of detection and limit of quantification for electrolyte-dimethyl carbonate(DMC),ethyl methyl carbonate(EMC)and diethyl carbonate(DEC)are 1.57-2.27μg/m^(3) and 4.99-7.23μg/m^(3),respectively.The results show a good linearity in the concentration range of 7.85-5270μg/m^(3) and 5078-89167μg/m^(3) with the coefficient(R2)greater than 0.997,and the recovery of standard addition is between 84.21%and 103.21%.When the pressure in the vacuum-assisted volatilization system is set to−27 kPa,the duration of a single detection is less than 8 min.To further verify the practicality of the method,a microleakage simulation system was developed and used in microleakage detection experiments on two types of 18650 and 21700 cylindrical lithium batteries.The results demonstrated that the detection method possesses the capacity to swiftly and accurately detect microleakage in lithium batteries.The method has the advantages of simple

关 键 词：真空辅助挥发装置 吸附/热脱附 气相色谱-质谱(GC-MS) 锂电池 挥发性有机物(VOCs) 

分 类 号：O657.63[理学—分析化学]