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EC 1206 0.890 8.36 × 10 −2.98 × 10 0.9831 Energies 2022, 15, 2805 3.2. LOD and LOQ of the GC×GC/FID method As shown in Figure 3, the minimum concentration of all the carbonate solvents, i.e., DMC, EMC, DEC, VC, PC, and EC, visually detected by the GC×GC/FID method was 0.2% 0.098, and 0.106 ppm in acetone for DMC, EMC, DEC, VC, PC, and EC, respectively. Fiiggurree33..GC×GC/FFIDIDcchhroromaatotoggraramooff00.2.2%%(v(v/v/)vs)osloultuiotinonofoDf DMMC,CE,MEMC,CD,EDCE,CV,CV,CP,CP,Ca,nadndECECin iancaectoetnoen.e. at a signal to noise ratio of 50, corresponding to injections of 0.084, 0.080, 0.077, 0.110, The statistical LOD and LOQ were determined using Equations (1) and (2), respec- The visual LOD, statistical LOD, and statistical LOQ are summarized in Table 4. EC and tively. The visual LOD, statistical LOD, and statistical LOQ are summarized in Table 4. EMC have the highest and lowest LOD and LOQ, respectively. These LODs are much lower EC and EMC have the highest and lowest LOD and LOQ, respectively. These LODs are than the LODs reported for one-dimensional gas chromatography with FID [13]. The LOQ much lower than the LODs reported for one-dimensional gas chromatography with FID for EMC, DEC, DMC, VC, PC, and EC were 3.04, 3.60, 4.23, 11.43, 12.13, and 16.41 ppm, [13]. The LOQ for EMC, DEC, DMC, VC, PC, and EC were 3.04, 3.60, 4.23, 11.43, 12.13, 8 of 14 The statistical LOD and LOQ were determined using Equations (1) and (2), respectively. respectively. and 16.41 ppm, respectively. Table 4. Limit of detection (LOD) and limit of quantification (LOQ) of DMC, EMC, DEC, VC, PC, Table 4. Limit of detection (LOD) and limit of quantification (LOQ) of DMC, EMC, DEC, VC, PC, and EC when using GC×GC/FID. and EC when using GC×GC/FID. Compound Statistical LOD Compound Visual LOD (ppm) Statistical LOD (ppm) LOQ (ppm) DMC 0.08 1.40 4.23 Visual LOD (ppm) (ppm) LOQ (ppm) DMC 0.08 1.40 4.23 EMC 0.08 1.00 3.04 EMC 0.08 1.00 3.04 DEC 0.08 1.19 3.60 DEC 0.08 1.19 3.60 VC 0.11 3.77 11.43 PC 0.10 4.00 12.13 VC 0.11 3.77 11.43 PC ECEC 0.10 0.101.11 4.00 5.451.41 12.13 16.1461.41 3..3..TeessttininggtthheeAcccuurraaccyyooffththeeIdIdeenntitfiifcicaatitoionnaannddQQuuaanntittiatatitoionnoof fCCaarbrboonnaatetsesbbyyUUsisningg GC×GC/EI TOF MS GC×GC/EI TOF MS Figure 4 shows the electron ionization (EI) mass spectra obtained by using GC×GC/EI Figure 4 shows the electron ionization (EI) mass spectra obtained by using GC×GC/EI TOF MS for DMC, EMC, DEC, VC, PC, and EC in the 100% calibration solution. The TOF MS for DMC, EMC, DEC, VC, PC, and EC in the 100% calibration solution. The sim- similarity factors upon comparison of the measured mass spectra to mass spectral libraries ilarity factors upon comparison of the measured mass spectra to mass spectral libraries for DMC, EMC, DEC, VC, PC, and EC were 864, 808, 941, 888, 895, and 929, respectively. for DMC, EMC, DEC, VC, PC, and EC were 864, 808, 941, 888, 895, and 929, respectively. Table 5 summarizes the retention times as well, as the slopes and the y-intercepts of the Table 5 summarizes the retention times as well, as the slopes and the y-intercepts of the calibration plots for each carbonate. Correlation coefficients for the linear regression of calibration plots for each carbonate. Correlation coefficients for the linear regression of GC×GC/EI TOF MS peak area to compound concentration ranged from 0.9533 for DMC GC×GC/EI TOF MS peak area to compound concentration ranged from 0.9533 for DMC to 0.9990 for PC. to 0.9990 for PC. Table 5. GC×GC/EI TOF MS calibration results, including the retention times and linear correlation parameters for common organic solvents found in Li-ion batteries. Compound DMC EMC DEC VC PC EC 1D-RT (s) 357 467 636 665 1526 1502 2D-RT (s) 1.64 1.85 2.05 1.79 1.77 1.71 Slope 1.82 × 106 2.23 × 106 2.43 × 106 3.15 × 106 1.50 × 106 1.72 × 106 Y-Intercept 5.75 × 104 −1.27 × 104 −6.25 × 103 6.05 × 104 3.22 × 103 −6.01 × 104 R2 0.9533 0.9547 0.9606 0.9943 0.9990 0.9981PDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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