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Figure 10. TIC and Mass Spectrum at Pyrolysis Region of PBA Using TDP/DART-MS
Py-GC/MS enables identification of polymer type using the available spectral library of pyrolysis products [4] (e.g. F-Search, Frontier Lab), (Figure 8).
MALDI-MS enables identification of polymer type using the observed mass interval corresponding to the mass of the repeating unit or the elemental compositions calculated from the mass (Figure 9).
TDP/DART-MS enables identification of polymer type without spectral library using the observed elemental compositions of the repeating unit (Figure 10).
Molecular weight distribution Figure 7. Mass Spectra at 450°C
In the mass spectra of the 0 km sample, the base oil was mainly detected. At 1,000 km, glycol compounds were also detected, and at 5,000 km, the glycol compounds were remarkably increased. In addition, the spectral pattern of the base oil compounds changed with the increase in mileage. Thus, these spectra provide information on the degradation state of base oil. By using this analysis method, it is clear that structural information for additives and base oil in automotive engine oils can be detected without any pretreatment of the samples. In addition, since it is possible to analyse structural information of additives and base oils in degraded automotive engine oils, this technique can be applied to evaluate the degradation degree of automotive engine oils and maintenance of machinery equipment.
Polymer Poly(butyl acrylate), PBA (Sigma Aldrich) was analysed by Py-GC/MS (Pyrolyzer: PY-2020iD, Frontier Lab, GC/MS: QP2010, Shimadzu, 6890GC/5975MSD, Agilent), MALDI-MS (autoflex speed, Bruker), and TDP/DART-MS (TDP: ionRocket, BioChromato, Ion Source: DART-SVP, IonSense, MS: Compact, Bruker) for the characterisation of the repeating unit, molecular weight distribution, and terminal functional groups.
Repeating Unit Figure 11b. SEC Curve for PBA
Figure 11a. Mass Spectra of PBA Using MALDI-MS (liner mode)
Figure 8. Pyrogram and Peak Assignment Table of PBA using Py-GC/MS
Figure 9. Mass Spectra of PBA Using MALDI-MS (reflector mode)
Figure 12. Mass Spectra of PBA Using SEC/MALDI-MS
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