Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal

In this work, two methods were investigated for determining the composition of carbonate solvent systems used in lithium-ion (Li-ion) battery electrolytes. One method was based on comprehensive two-dimensional gas chromatography with electron ionization time-of-flight mass spectrometry (GC×GC/EI TOF...

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Main Authors: Mohammad Parhizi, Louis Edwards Caceres-Martinez, Brent A. Modereger, Hilkka I. Kenttämaa, Gozdem Kilaz, Jason K. Ostanek
Format: Article
Language:English
Published: MDPI AG 2022-04-01
Series:Energies
Subjects:
Online Access:https://www.mdpi.com/1996-1073/15/8/2805
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author Mohammad Parhizi
Louis Edwards Caceres-Martinez
Brent A. Modereger
Hilkka I. Kenttämaa
Gozdem Kilaz
Jason K. Ostanek
author_facet Mohammad Parhizi
Louis Edwards Caceres-Martinez
Brent A. Modereger
Hilkka I. Kenttämaa
Gozdem Kilaz
Jason K. Ostanek
author_sort Mohammad Parhizi
collection DOAJ
description In this work, two methods were investigated for determining the composition of carbonate solvent systems used in lithium-ion (Li-ion) battery electrolytes. One method was based on comprehensive two-dimensional gas chromatography with electron ionization time-of-flight mass spectrometry (GC×GC/EI TOF MS), which often enables unknown compound identification by their electron ionization (EI) mass spectra. The other method was based on comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC/FID). Both methods were used to determine the concentrations of six different commonly used carbonates in Li-ion battery electrolytes (i.e., ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), ethyl methyl carbonate (EMC), and vinylene carbonate (VC) in model compound mixtures (MCMs), single-blind samples (SBS), and a commercially obtained electrolyte solution (COES). Both methods were found to be precise (uncertainty < 5%), accurate (error < 5%), and sensitive (limit of detection <0.12 ppm for FID and <2.7 ppm for MS). Furthermore, unlike the previously reported methods, these methods do not require removing lithium hexafluorophosphate salt (LiPF<sub>6</sub>) from the sample prior to analysis. Removal of the lithium salt was avoided by diluting the electrolyte solutions prior to analysis (1000-fold dilution) and using minimal sample volumes (0.1 µL) for analysis.
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spelling doaj.art-00599d966ef648de81e5fe68527f83862023-12-01T20:48:46ZengMDPI AGEnergies1996-10732022-04-01158280510.3390/en15082805Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt RemovalMohammad Parhizi0Louis Edwards Caceres-Martinez1Brent A. Modereger2Hilkka I. Kenttämaa3Gozdem Kilaz4Jason K. Ostanek5School of Engineering Technology, Purdue University, 401 N. Grant St., West Lafayette, IN 47907, USASchool of Engineering Technology, Purdue University, 401 N. Grant St., West Lafayette, IN 47907, USADepartment of Chemistry, Purdue University, 560 Oval Dr., West Lafayette, IN 47907, USADepartment of Chemistry, Purdue University, 560 Oval Dr., West Lafayette, IN 47907, USASchool of Engineering Technology, Purdue University, 401 N. Grant St., West Lafayette, IN 47907, USASchool of Engineering Technology, Purdue University, 401 N. Grant St., West Lafayette, IN 47907, USAIn this work, two methods were investigated for determining the composition of carbonate solvent systems used in lithium-ion (Li-ion) battery electrolytes. One method was based on comprehensive two-dimensional gas chromatography with electron ionization time-of-flight mass spectrometry (GC×GC/EI TOF MS), which often enables unknown compound identification by their electron ionization (EI) mass spectra. The other method was based on comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC/FID). Both methods were used to determine the concentrations of six different commonly used carbonates in Li-ion battery electrolytes (i.e., ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), ethyl methyl carbonate (EMC), and vinylene carbonate (VC) in model compound mixtures (MCMs), single-blind samples (SBS), and a commercially obtained electrolyte solution (COES). Both methods were found to be precise (uncertainty < 5%), accurate (error < 5%), and sensitive (limit of detection <0.12 ppm for FID and <2.7 ppm for MS). Furthermore, unlike the previously reported methods, these methods do not require removing lithium hexafluorophosphate salt (LiPF<sub>6</sub>) from the sample prior to analysis. Removal of the lithium salt was avoided by diluting the electrolyte solutions prior to analysis (1000-fold dilution) and using minimal sample volumes (0.1 µL) for analysis.https://www.mdpi.com/1996-1073/15/8/2805lithium-ion batterieselectrolytetwo-dimensional gas chromatography (GC×GC)mass spectrometry (MS)flame ionization detector (FID)analytical techniques
spellingShingle Mohammad Parhizi
Louis Edwards Caceres-Martinez
Brent A. Modereger
Hilkka I. Kenttämaa
Gozdem Kilaz
Jason K. Ostanek
Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
Energies
lithium-ion batteries
electrolyte
two-dimensional gas chromatography (GC×GC)
mass spectrometry (MS)
flame ionization detector (FID)
analytical techniques
title Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
title_full Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
title_fullStr Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
title_full_unstemmed Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
title_short Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal
title_sort determining the composition of carbonate solvent systems used in lithium ion batteries without salt removal
topic lithium-ion batteries
electrolyte
two-dimensional gas chromatography (GC×GC)
mass spectrometry (MS)
flame ionization detector (FID)
analytical techniques
url https://www.mdpi.com/1996-1073/15/8/2805
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