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Energies 2022, 15, x FOR PEER REVIEW 9 of 14 Energies 2022, 15, 2805 9 of 14 Figure 4. 70 eV EI mass spectra obtained by using GC×GC/EI TOF MS for DMC, EMC, DEC, VC, Figure 4. 70 eV EI mass spectra obtained by using GC×GC/EI TOF MS for DMC, EMC, DEC, VC, PC, and EC. PC, and EC. Table 5. GC×GC/EI TOF MS calibration results, including the retention times and linear correlation 3.4. LOD and LOQ of the GC×GC/EI TOF MS Method parameters for common organic solvents found in Li-ion batteries. Carbonates in the solutions with the lowest concentrations, i.e., 0.1%, 0.2%, 0.4%, 0.6%, Compound 1D-RT (s) 2D-RT (s) Slope Y-Intercept R2 and 0.8% (v/v) were not detected by GC×GC/EI TOF MS. The minimum concentration DMC 357 1.64 1.82 × 106 5.75 × 104 0.9533 (v/v) detected was for the 1% calibration solution (corresponding to injection of 0.42, 0.40, EMC 467 1.85 2.23 × 106 −1.27 × 104 0.9547 0.39, and 0.55 ppm of DMC, EMC, DEC, and VC, respectively) or 5% (v/v) (corresponding DEC 636 2.05 2.43 × 106 −6.25 × 103 0.9606 to injection of 2.44 and 2.66 ppm of PC, and EC, respectively). The LOD and LOQ for VC 665 1.79 3.15 × 106 6.05 × 104 0.9943 the GC×GC/EI TOF MS method are summarized in Table 6. The statistical LOD was the 63 greatesPtfCorDMC,EM1C5,2D6EC,andVC1.7a7ndlower1fo.5r0P×C1a0ndEC.S3ta.2ti2st×ic1a0lLODw0a.s99lo9w0er 64 than thEeCvisual LOD fo1r50P2C and EC. N1.o71solutions1w.7e2re×p1r0epared a−t6c.o0n1c×en10trations0b.e9t9w81een 1–5% for PC and EC. The LODs and LOQs were generally lower for the GC×GC/FID method than they were for the GC×GC/EI TOF MS method. 3.4. LOD and LOQ of the GC×GC/EI TOF MS Method Carbonates in the solutions with the lowest concentrations, i.e., 0.1%, 0.2%, 0.4%, Table 6. Limit of detection (LOD) and limit of quantification (LOQ) for DMC, EMC, DEC, VC, PC, 0.6%, and 0.8% (v/v) were not detected by GC×GC/EI TOF MS. The minimum concentra- and EC obtained using the GC×GC/EI TOF MS method. tion (v/v) detected was for the 1% calibration solution (corresponding to injection of 0.42, 0.40, 0.39, and 0.55 ppm of DMC, EMC, DEC, and VC, respectively) or 5% (v/v) (corre- Compound Visual LOD (ppm) Statistical LOD LOQ (ppm) sponding to injection of 2.44 and 2.66 ppm of PC, a(npdpmE)C, respectively). The LOD and LOQ for the GC×GC/EI TOF MS method are summarized in Table 6. The statistical LOD DMC 0.42 6.58 19.95 was the greatest for DMC, EMC, DEC, and VC and lower for PC and EC. Statistical LOD EMC 0.40 6.92 20.97 was loweDrEtChan the visual LOD0f.o3r9 PC and EC. No sol5u.5ti6ons were prepared1a6t.8c4oncentra- VC 0.55 3.23 9.80 tions between 1–5% for PC and EC. The LODs and LOQs were generally lower for the PC 2.44 1.55 4.70 GC×GC/FID method than they were for the GC×GC/EI TOF MS method. EC 2.66 2.05 6.21PDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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