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Energies 2022, 15, 2805 10 of 14 3.5. Testing the Accuracy of the Quantitation of MCMs The intraday repeatability of quantitation was determined for both methods by mea- suring three samples that were prepared in the same way but on different days. The compositions determined for MCM #1A, MCM #1B, and MCM #1C are shown in Table 7. The results for MCM #1A-C were similar. The average volume percentage determined using GC×GC/FID for DMC, DEC, EMC, VC, and PC were 19.6 ± 2.4, 20.5 ± 1.5, 19.3 ± 0.8, 19.3 ± 3.1, and #20.9 ± 1.9% (v/v), respectively. The average volume percentage determined using GC×GC/EI TOF MS for DMC, DEC, EMC, VC, and PC were 17.0 ± 1.5, 20.2 ± 1.3, 21.6 ± 1.6, 20.1 ± 1.4, and 19.8 ± 1.9% (v/v), respectively. Measurements made on the same day were similar to each other (average relative standard deviation = 3.9%). In general, both instruments predicted the volume percentages of the carbonates with good accuracy. The largest error for the GC×GC/FID method was observed for PC, and the largest error observed for the GC×GC/EI TOF MS method was associated with DMC. Table 7. Volume fraction of the components in MCM #1A-C measured using GC×GC/FID and GC×GC/EI TOF/MS. The expected concentration of each carbonate was 20 ± 1.5% for MCM#1A–C. Volume Percentages MCM #1 MCM Injection DMC % MS FID DEC % MS FID 19.9 20.1 20.5 20.6 20.4 20.5 19.9 20.6 19.9 20.6 19.5 20.8 20.4 20.7 20.6 20.6 20.3 20.3 EMC % MS FID 21.0 17.1 21.5 17.6 20.9 20.6 22.1 19.9 21.9 20.4 21.6 19.7 22.4 19.1 21.5 19.1 21.4 20.1 VC % MS FID 20.0 19.1 20.5 19.8 20.0 18.0 19.8 21.0 19.7 21.4 19.3 18.6 20.2 18.4 20.8 18.6 21.0 18.5 PC % MS FID 20.2 17.4 20.8 17.7 20.1 17.7 19.5 23.3 19.5 23.3 19.4 23.8 20.2 22.2 19.5 21.6 19.3 21.2 #1A 2 #1B 2 #1C 2 1 17.2 19.5 17.2 20.2 3 17.2 19.2 1 16.9 19.2 17.3 19.4 3 17.0 19.2 1 17.1 20.0 16.6 19.9 3 16.9 19.9 Additional MCMs were also analyzed using GC×GC/FID. The compositions deter- mined for MCM #2 and MCM #3 are shown in Figure 5. MCM #2 was 20, 20, and 60% EMC, VC, and DMC, respectively. MCM #3 was 60, 20, and 20% EC, DEC, and PC, respectively. The uncertainties associated with the measurement of each compound and the actual con- centration are also shown in Figure 5. The percentage errors of the GC×GC/FID method for EMC, VC, and EC in MCM #2, were 1.1, 0.7, 0.4%, respectively (average percentage error = 0.7%). The percentage errors of the GC×GC/FID method for EC, DEC, and PC in MCM #3, were 2.6, 3.1, 2.8%, respectively (average percentage error = 2.8%). Furthermore, Energies 2022, 15, x FOR PEER REVIEW 11 of 14 the greatest uncertainty associated with the measurements was 4.1% for DMC in MCM #2, and 4.3% for EC in MCM #3. Figure 5. Expected and measured volume percentages of carbonates in MCM #2 (a) and MCM #3 Figure 5. Expected and measured volume percentages of carbonates in MCM #2 (a) and MCM #3 (b) (b) determined with GC×GC/FID. determined with GC×GC/FID. 3.6. Testing the Accuracy of Quantitation of SBSs and COES The compositions determined for SBSs and COES are shown in Figure 6. The errors in the expected volume percentages of the electrolytes in SBS #2 (which was prepared with a commercially obtained electrolyte solution as described in the experimental section) and the COES were especially large because of large uncertainties mentioned in the product specifications from the manufacturer. Both methods were very accurate. The percentage errors of the GC×GC/FID method for EC, EMC, and VC in SPS #1 were 0.8, 1.0, and 0.4%,PDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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