气相色谱-质谱联用法检测电解质组分方法优化

刘媛丽; 岳金明; 李泉; 陈一霞

doi:10.19799/j.cnki.2095-4239.2026.0397

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气相色谱-质谱联用法检测电解质组分方法优化

储能测试与评价 | 更新时间：2026-09-18

- 气相色谱-质谱联用法检测电解质组分方法优化
- Optimization of gas chromatography mass spectrometric detection method for electrolyte
- 储能科学与技术 2026年15卷第9期页码：3738-3749
- 作者机构：
  
  中国科学院物理研究所，北京 100190
- 作者简介：
  
  刘媛丽（1989—），女，本科，工程师，主要从事锂离子电池电解液分析测试，E-mail：liuyuanli@iphy.ac.cn；
  李泉，副研究员，主要从事高能量密度固态电池研究，E-mail：qli@iphy.ac.cn。
- 基金信息：
  
  中国科学院B类先导项目(XDB 1040401);国家自然科学基金(22409213;92572301)
- DOI：10.19799/j.cnki.2095-4239.2026.0397
  中图分类号： TM 912
- 收稿：2026-05-09，
  
  修回：2026-07-03，
  
  纸质出版：2026-09-28
- 稿件说明：
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刘媛丽, 岳金明, 李泉, 等. 气相色谱-质谱联用法检测电解质组分方法优化[J]. 储能科学与技术, 2026, 15(9): 3738-3749.

LIU Yuanli, YUE Jinming, LI Quan, et al. Optimization of gas chromatography mass spectrometric detection method for electrolyte[J]. Energy Storage Science and Technology, 2026, 15(9): 3738-3749.
刘媛丽, 岳金明, 李泉, 等. 气相色谱-质谱联用法检测电解质组分方法优化[J]. 储能科学与技术, 2026, 15(9): 3738-3749. DOI： 10.19799/j.cnki.2095-4239.2026.0397.

LIU Yuanli, YUE Jinming, LI Quan, et al. Optimization of gas chromatography mass spectrometric detection method for electrolyte[J]. Energy Storage Science and Technology, 2026, 15(9): 3738-3749. DOI： 10.19799/j.cnki.2095-4239.2026.0397.

摘要

电解质是锂离子/固态电池的核心组成部分，为锂离子在正负极之间往返迁移提供媒介，并参与形成保护电极的界面膜，是决定电池能量密度、寿命、安全及高低温性能的关键。对于原位固态化技术，固化前的单体和溶剂是提升性能的关键组分，添加量的精准控制直接影响电池性能与成本。然而，针对双氟代碳酸乙烯酯（DFEC）这类痕量级添加剂，现有检测方法面临挑战：痕量DFEC与结构类似物甲基三氟乙基碳酸酯（FEMC）在色谱上保留相似，难以基线分离；在复杂基质下的痕量DFEC信号易被掩盖，存在检出限高、精密度差等技术瓶颈。对此，针对气相色谱-质谱联用（GC-MS）技术在相似物质上难以分离的问题，以痕量DFEC为例建立标准化的检测方法，通过对提取溶剂和仪器参数的系统优化，实现了痕量DFEC的准确检测及其与FEMC的有效分离。结果表明，该方法在0.8～160 μg/mL范围内线性关系良好（相关系数

0.999），检出限（LOD）达0.25 μg/mL，不同浓度水平下的加标回收率为95.1%～105.7%，精密度良好（相对标准偏差RSD小于2%），所建立的方法准确度高、重复性良好，为电解质体系的同系物分离与痕量组分检测，原位固化电解液配方设计与电池机理的深入研究提供可靠的技术支持。

Abstract

As the core component of solid-state batteries

the electrolyte serves as the medium for lithium-ion transport between the cathode and anode

participates in the formation of protective interfacial films on the electrodes

and plays a crucial role in determining battery energy density

cycle life

safety

and high- and low-temperature performance. Although the monomer and solvent constitute only a minor fraction of the

situ

solidified electrolyte

accurately measuring and controlling their concentrations is critical for optimizing battery performance

reducing cost

and enhancing safety. However

existing analytical methods face considerable challenges in quantifying trace-level additives such as bis(fluoroethylene carbonate) (DFEC). Trace DFEC and its structural analog

methyl trifluoroethyl carbonate (FEMC)

hibit similar chromatographic retention behavior

making baseline separation difficult. Moreover

the signal of trace DFEC is readily masked in complex matrices

leading to technical bottlenecks including high detection limits and poor precision. To address the challenge of separating structurally similar compounds via gas chromatography-mass spectrometry

this study uses trace DFEC as a model analyte to establish a standardized analytical method. Through systematic screening of extraction solvents and optimization of instrumental parameters

accurate detection of trace DFEC and its effective separation from FEMC were achieved. The optimized method showed excellent linearity (

0.999) over the concentration range of 0.8—160 μg/mL. The limit of detection was 0.25 μg/mL

recoveries ranged from 95.1% to 105.7%

and the method demonstrated good precision

with relative standard deviations of

2%. The established method provides high accuracy

excellent repeatability

and reliable technical support for the separation of structurally related compounds and the detection of trace components in electrolyte systems. It also provides a robust analytical foundation for the formulation design of

situ

solidified electrolytes and for in-depth investigations of battery mechanisms.

关键词

Keywords

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