Carbonate Solvent Systems Used in Lithium-Ion Batteries

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Carbonate Solvent Systems Used in Lithium-Ion Batteries ( carbonate-solvent-systems-used-lithium-ion-batteries )

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= +(∙) = +(∙) (5) Energies 2022, 15, 2805 as x = (y − b)/m. Note that y is the measured peak area with a precision index (random 7 of 14 where t was the student’s multiplier for 95% confidence, which for N = 3, 5, and 10, was 4.303, 2.776, 2.365, 2.262 [23]. From the calibration curves, the concentration of each compound can be determined error), b is the intercept with fixed errors, and m is the slope with fixed errors. Therefore, the fixed and random error associated with concentration, x, can be determined as follows: error), b is the intercept with fixed errors, and m is the slope with fixed errors. Therefore, = + = (6) the fixed and random error associated with concentration, x, can be determined as follows: The total uncertainty􏲭associated with concentration of a c􏲭ompound, x, can be written as: 􏰎 ∂x 􏰏2 BR = URm as: 3. Results and Discussion 􏰏2 􏰎∂x SR = 􏰏2 􏰎∂x ∂m ∂b ∂y + Sy The total uncertainty associated with concentration of a compound, x, can be written URb (6) (7) Ux =􏲬B2 +􏱨t×S 􏱩2 (7) RR =+(×) 3.1. Testing the Accuracy of Identification and Quantitation of Carbonates by Using 3. Results and Discussion GC×GC/FID 3.1. Testing the Accuracy of Identification and Quantitation of Carbonates by Using GC×GC/FID Carbonate compounds were identified using GC×GC/FID, based on their first- and Carbonate compounds were identified using GC×GC/FID, based on their first- and second-dimension retention times (1D-RT and 2D-RT) of each carbonate. Figure 2 shows second-dimension retention times (1D-RT and 2D-RT) of each carbonate. Figure 2 shows a a three-dimensional chromatogram obtained by using GC×GC/FID for the 100% calibra- three-dimensional chromatogram obtained by using GC×GC/FID for the 100% calibration tion solution. All the compounds were completely separated by GC×GC, allowing each solution. All the compounds were completely separated by GC×GC, allowing each carbon- carbonate to be detected without interference from the others. Table 3 summarizes the ate to be detected without interference from the others. Table 3 summarizes the retention retention times as well as the slope and the Y-intercept for the calibration curve of each times as well as the slope and the Y-interc2ept for the calibration curve of each carbonate. carbonate. Linear correlation coefficients (R ) were found to be greater than 0.977 for all Linear correlation coefficients (R2) were found to be greater than 0.977 for all cases. cases. Figure 2. Three-dimensional chromatogram exhibiting effective separation of the carbonates in the Figure 2. Three-dimensional chromatogram exhibiting effective separation of the carbonates in the 10100%0%cacliablirbartaiotinonsosloultuiotinonwwhehnenusuinsigngthtehGe CG×CG×CG/FCI/DFsIDyssteymste. m. Table 3. GC×GC/FID calibration results including the retention times and linear correlation param- Table 3. GC×GC/FID calibration results including the retention times and linear correlation parame- eters for common organic solvents found in Li-ion batteries. ters for common organic solvents found in Li-ion batteries. Compound 1D-RT (s) 2D-RT (s) Slope Y-Intercept 2 R2 Compound 1D-RT (s) 2D-RT (s) Slope Y-Intercept R DMC 171 171 0.695 9.82 × 107 −7.79 × 105 0.9987 DMC 0.695 9.82 × 107 1.89 ×8 108 −7.79 × 105 −7.07 × 1505 0.9987 EMC 240 1.160 1.89 × 10 2.00 ×8 108 −7.07 × 10 −4.17 × 1606 0.9970 EMC 240 1.160 0.9970 DEC 351 1.740 2.00 × 10 −4.17 × 10 66 0.9952 DEC 351 1.740 0.9952 0.9867 VVCC 1.0815.085 77 PC 1.090 1.38 × 108 2.27 × 106 2.27 × 10 −2.98 × 105 0.9774 PC 1194 1.090 1.38 × 10 8 6 0.9774 EC 1206 0.890 8.36 × 107 0.9831 408408 1194 9.099×.0910× 10 −1−.513.5×3 1×010 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% at a signal to noise ratio of 50, corresponding to injections of 0.084, 0.080, 0.077, 0.110, 0.098, and 0.106 ppm in acetone for DMC, EMC, DEC, VC, PC, and EC, respectively.

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