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Energies 2022, 15, 2805 12 of 14 3.7. Analysis of Column Bleeding before and after Salt Injection To determine whether the samples containing LiPF6 salt cause excessive column bleeding, an experiment was conducted by injecting a blank acetone sample (considered as the baseline sample) before and after five injections of COES and SBS #2. Figure 7 shows the GC×GC-FID/chromatograms of acetone before and after injection of salt-containing samples. No changes were observed in the amount of column bleeding, noise, or retention times before and after samples that contained LiPF6 were analyzed, which suggests that the effects of the LiPF6 on the GC columns were negligible. The solvent-bleeding also remained Fuingcuhrean6.gVedol.ume percentages determined for carbonates in SBS #1 (a), SBS #2 (b), and COES (c). Figure 7. GC×GC/FID chromatograms of acetone before (a) and after (b) ten samples containing Figure 7. GC×GC/FID chromatograms of acetone before (a) and after (b) ten samples containing LiPF6 were analyzed. LiPF6 were analyzed. As shown in Figure 8, no additional column bleeding or changes in retention times As shown in Figure 8, no additional column bleeding or changes in retention times or peak shapes were observed for COES or SBS #2, which further suggests that the effects or peak shapes were observed for COES or SBS #2, which further suggests that the effects of the LiPF6 salt were negligible. This is likely because very little salt was introduced into of the LiPF6 salt were negligible. This is likely because very little salt was introduced into the instrument (samplles were diluted 1000--ffolld priiorr tto anallysiis,, and onlly 0..1 μL of the liners were replaced when needed. diluted samples was analyzed). Additionally, inlet liners with glass wool were used at the Energies 2022, 15, x FOR PEER REVIEW 13 of 14 inlet of the GC×GCiinssttrrumeenttsstto ttrap nonvollattiille compounds,, such as LiPF6,, and the 6 (a) (b) Figure 8. GC×GC/FID chromatograms of salt-containing samples: (a) COES and (b) SBS #2. Figure 8. GC×GC/FID chromatograms of salt-containing samples: (a) COES and (b) SBS #2. 44..CCoonncclulussioionnss TTwoomethodsareddeessccrriibbeedtotodedtetremrminienethtehceomcopmopsiotsioitnioonfcoafrbcaornbaotneastoelvseonlvtesnyts- styesmtesmcsocmomomnolynluysuesdedininLiL-iio-inonbabtatettreyryelelcetcrtorloyltyetesosloulutitoionns,so, onneebbaaseseddoonnGC×GC/FFIID aannddaannootthheerrbaasseedonGC×GGCC/E/IETIOTOFFMMS.ST. Theheacacucurarcaycyananddpprerecicsiisoionnooffththeemeetthhooddss weerreetteesstteedussininggvaarrioiouussmooddeellccoomppoouunnddmixixtuturreess((MCMss),),aaccoommeerrcciaiallylyoobbtatainineedd eelelecctrtroolylytetessoolulutitoionn(C(COEESS),),aannddssiningglele-b-blilninddssaamppleless((SSBBSSss).).BBooththmeeththooddssweerreeffoouunndd to be accurate, precise, and sensitive. The high sensitivity of the methods allowed the use to be accurate, precise, and sensitive. The high sensitivity of the methods allowed the use of high dilution factors and low injection volumes, eliminating the need for salt removal. of high dilution factors and low injection volumes, eliminating the need for salt removal. No adverse effects on column bleeding, retention times, or GC peak shapes were observed No adverse effects on column bleeding, retention times, or GC peak shapes were observed whileanalyzingsamplescontainingLiPF salt.Themethodsemployedinthisstudywill while analyzing samples containing LiPF66salt. The methods employed in this study will be used in future studies to investigate changes in the composition of electrolyte solutions be used in future studies to investigate changes in the composition of electrolyte solutions from Li-ion batteries over time, after calendar aging, and after cycle aging. from Li-ion batteries over time, after calendar aging, and after cycle aging. Author Contributions: Conceptualization, G.K. and J.K.O.; methodology, M.P., L.E.C.-M., B.A.M., H.I.K., G.K. and J.K.O.; formal analysis, M.P., L.E.C.-M. and B.A.M.; investigation, M.P., L.E.C.-M. and B.A.M.; resources, H.I.K., G.K. and J.K.O.; data curation, M.P., L.E.C.-M. and B.A.M.; writing— original draft preparation, M.P., L.E.C.-M. and B.A.M.; writing—review and editing, M.P., L.E.C.- M., B.A.M., H.I.K., G.K. and J.K.O.; visualization, M.P.; supervision, H.I.K., G.K. and J.K.O.; project administration, H.I.K., G.K. and J.K.O.; funding acquisition, G.K. and J.K.O. All authors have readPDF Image | Carbonate Solvent Systems Used in Lithium-Ion Batteries
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