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Energies 2022, 15, 2805 5 of 14 solutions corresponding to 1, 5, 10, 20, 40, 60, and 80% (v/v) used for calibration. The stock solution was prepared by dissolving 200 μL of DMC, DEC, PC, EMC, VC, and 264.2 mg of EC (equivalent to 200 μL considering ρEC = 1.321 g/cm3) in 200 mL of acetone. Each calibration curve solution was then analyzed with GC×GC/FID and GC×GC/EI TOF MS according to Sections 2.3 and 2.4, respectively. The concentration of each carbonate in each calibration curve solution is shown in Table 2. In addition, each of the calibration curve solutions was analyzed five times with GC×GC/FID and five times with GC×GC/EI TOF MS. SBSs, MCMs, and COES were analyzed 10 times each with GC×GC/FID and ten times each with GC×GC/EI TOF MS. Table 2. Concentrations of carbonates in calibration solutions. Calibration Solution 100% 80% 60% 40% 20% 10% 5% 1% DMC EMC 1045.0 1005.0 836.0 804.0 627.0 603.0 418.0 402.0 209.0 201.0 104.5 100.5 52.3 50.3 10.5 10.1 Concentration [ppm] DEC VC PC EC 965.0 1370.0 1221.0 1321.0 2.6. Identification and Quantitation of the Carbonates Testing the ability of GC×GC/FID to identify the carbonates was carried out by preparing samples of individual carbonates, i.e., 10 μL of DMC, DEC, PC, EMC, VC, and 13.21 mg of EC in 10 mL acetone, and injecting them separately into the GC×GC system to create a map for individual carbonates based on their first and second-retention times. Testing the GC×GC/EI TOF MS method was based on the comparison of the measured EI mass spectra to the EI mass spectral library. Testing the quantitation of DMC, DEC, PC, EMC, VC, and EC was carried out by exporting the peak areas for each carbonate in the calibration solutions after data processing in GC×GC/FID and GC×GC/EI TOF MS to Microsoft Excel 365. The slope and intercept associated with the calibration curve of each compound were then determined using conventional linear regression analysis. 2.7. LOD and LOQ The statistical LOD and LOQ for each compound was determined based on the standard deviation (σ) of the intercept over the slope (M) in the calibration curve data by using Equations (1) and (2), respectively [21]. σintercept LOD = 3.3 ∗ M (1) σintercept LOQ = 10.0 ∗ M (2) In order to accurately determine LOD and LOQ, additional solutions with lower concentrations, i.e., 0.1%, 0.2%, 0.4%, 0.6%, and 0.8% (v/v), were analyzed and data added to the original 8-point calibration curves. 2.8. Analysis of Column Bleeding Aiming to determine whether the samples containing LiPF6 salt cause excessive column bleeding, an experiment was carried out by injecting a blank acetone sample (considered as the baseline sample) before and after five injections of COES and SBS #2. All chromatograms were inspected for any visual signs of column bleed, changes in peak shapes, or changes in retention times. 772.0 1096.0 579.0 822.0 386.0 548.0 193.0 274.0 976.8 732.6 488.4 244.2 122.1 61.1 12.2 1056.8 792.6 528.4 264.2 132.1 66.1 13.2 96.5 48.3 9.7 137.0 68.5 13.7PDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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