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Energies 2022, 15, 2805 3 of 14 to food, petrochemical, environmental, biomedical, hardware, and software industries [20]. However, to the best of the authors’ knowledge, determination of the compositions of the solvent systems used in Li-ion battery electrolytes has not been performed based on GC×GC/FID or GC×GC/EI TOF MS. The purpose of the present work was to determine the accuracy and precision of these two analytical techniques when analyzing compounds found in electrolyte solutions of Li-ion batteries. To quantify and compare the performance of the two analytical techniques, the limit of detection (LOD), limit of quantification (LOQ), uncertainty, and repeatability were determined. 2. Experimental 2.1. Chemicals Ethylene carbonate (EC; ≥99%), propylene carbonate (PC; ≥99%), dimethyl carbonate (DMC; 99.9%), diethyl carbonate (DEC; ≥99%), ethyl methyl carbonate (EMC; 99.9%), viny- lene carbonate (VC; 99.5%), a commercially available Li-ion battery electrolyte comprised of a 1.0 M (±0.1 M) LiPF6 solution in 50/50 (v/v) (±5%) EC and DMC, a commercially available Li-ion battery electrolyte comprised of a 1.0 M (±0.1 M) LiPF6 solution in 50/50 (v/v) (±5%) EC and DEC, and a commercially available Li-ion battery electrolyte comprised of a 1.0 M (±0.1 M) LiPF6 solution in 50/50 (v/v) (±5%) EC and EMC were purchased from Sigma-Aldrich (St. Louis, MO, USA). Dichloromethane (DCM) (ACROS Organics; ≥99.9%) and acetone (Honeywell Burdick & Jackson; ≥99.9%) were purchased from Fisher Scientific (Branchburg, NJ, USA). Isopropanol (IPA; 99.8%) was purchased from Techspray (Kennesaw, GA, USA). All chemicals were used as received. 2.2. Carbonate Mixtures and Li-Ion Battery Electrolyte Various model mixtures of known carbonates were used to determine the accuracy and precision of the GC×GC/FID and GC×GC/EI TOF MS methods. Model compound mixtures (MCMs) with three different compositions were prepared and analyzed (MCM #1, MCM #2, and MCM #3; Table 1). One MCM was prepared and analyzed on three different days (MCM #1A MCM #2A, and MCM #3A; Table 1) to determine the intraday repeatability of the methods. A commercially obtained electrolyte solution (COES) of 1.0 M LiPF6 solu- tion in 50:50 (v/v) (±5%) EC and DMC was purchased from Sigma-Aldrich and analyzed using both methods (Table 1). Two single-blind samples (SBSs) were also analyzed (using both methods) that were prepared by members of a different laboratory with compositions that were revealed only after they were analyzed (SBS; Table 1). SBS #1 was prepared with pure EC (≥99%), EMC (≥99.9%), VC (≥99.5%), and isopropanol (IPA; 99.8%). SBS #2 was prepared from an electrolyte solution in 50:50 (v/v) (±5%) EC and EMC, an electrolyte solution in 50:50 (v/v) (±5%) EC and DEC, and pure VC (≥99.5%). SBS #1 and SBS#2 were shipped (~3 h) then stored (up to 6 months) prior to preparation and injection. Samples were prepared by diluting 10 μL of each mixture in 10 mL DCM or acetone. Each sample was injected 10 times into both instruments with an injection volume of 0.1 μL and a split ratio of 24. Table 1. Composition of various mixtures analyzed by GC×GC/FID and GC×GC/EI TOF MS methods. Mixture MCM #1A MCM #1B EC EMC DMC - 20.0 20.0 - 20.0 20.0 Volume Percentages % DEC PC 20.0 20.0 20.0 20.0 20.0 20.0 VC 20.0 20.0 LiPF6 IPA - - - - - - - - - - - 14.4 MCM#1C - MCM#2 - MCM #3 SBS #1 SBS #2 COES 20.0 20.0 20.0 60.0 20.0 - 20.0 - - 20.0 60.0 27.8 42.8 45.0 - 45.0 - 20.0 - 55 - 21.4 - - - 2.8 21.4-4.79.6- - - - 10.0 -PDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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