Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom
Characterization of aliphatic hyperbranched polyesters by MALDI-TOF mass spectrometry
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U okviru ovog rada prikazani su rezultati ispitivanja opsega sporednih proizvoda (ciklika) kod hidroksi-funkcionalnih alifatskih hiperrazgranatih poliestara primenom MALDI-TOF masene spektrometrije. Istovremeno su opisani i osnovni principi MALDI-TOF masene spektrometrije i dat je kratak literaturni pregled.
In this work, MALDI-TOF mass spectrometry was used for the characterization of aliphatic hyperbranched polyesters (AHBP), synthesized from 2,2-bis(hydroxymethyl)propionic acid (bis-MPA) and di-trimethylolpropane. From the obtained results it was concluded that it was not possible to take complete advantages of MALDI-TOF MS in this particular case, since the AHBP used in this work were polydisperse. The intensity of the signals from the high mass tail of these samples (pseudo generation higher than four) was underestimated and insufficient to distinguish it from the baseline and to use it for the analysis of the spectra. As a consequence of that, lower values of the Mn were obtained. At the same time, Mw were also underestimated, which led to very low values of the polydispersity index. On the other hand, it was possible to obtain molar masses of individual molecules from the MALDI-TOF mass spectra of AHBP and to qualitatively determine the extent of cyclization (side reactions) at each... degree of polymerization. Using the adequate set of equations and results obtained from MALDI-TOF mass spectra of AHBP, every signal from the spectra was identified. The obtained results show that formation of poly(bis-MPA), intramolecular esterification and intramolecular etherification occurred as side reactions during the synthesis of these polyesters. The relative amount of the cycles increases with the number of pseudo generation (from the second up to the fifth pseudo generation). It was also observed that the relative proportion of the signals which represent cyclic structures increases with the increasing degree of polymerization. In this work the basic principles of MALDI-TOF MS are also presented, as well as, a review of adequate published articles.
Кључне речи:
MALDI-TOF MS / alifatski hiperrazgranati poliestri / aliphatic hyperbranched polyestersИзвор:
Hemijska Industrija, 2007, 61, 6, 333-341Издавач:
- Association of Chemical Engineers of Serbia,
Напомена:
- Ovo je rad Jasne Džunuzović.
Институција/група
IHTMTY - JOUR AU - Vuković, Jasna AU - Jovanović, Slobodan AU - Lechner, Manfred D. PY - 2007 UR - https://cer.ihtm.bg.ac.rs/handle/123456789/6890 AB - U okviru ovog rada prikazani su rezultati ispitivanja opsega sporednih proizvoda (ciklika) kod hidroksi-funkcionalnih alifatskih hiperrazgranatih poliestara primenom MALDI-TOF masene spektrometrije. Istovremeno su opisani i osnovni principi MALDI-TOF masene spektrometrije i dat je kratak literaturni pregled. AB - In this work, MALDI-TOF mass spectrometry was used for the characterization of aliphatic hyperbranched polyesters (AHBP), synthesized from 2,2-bis(hydroxymethyl)propionic acid (bis-MPA) and di-trimethylolpropane. From the obtained results it was concluded that it was not possible to take complete advantages of MALDI-TOF MS in this particular case, since the AHBP used in this work were polydisperse. The intensity of the signals from the high mass tail of these samples (pseudo generation higher than four) was underestimated and insufficient to distinguish it from the baseline and to use it for the analysis of the spectra. As a consequence of that, lower values of the Mn were obtained. At the same time, Mw were also underestimated, which led to very low values of the polydispersity index. On the other hand, it was possible to obtain molar masses of individual molecules from the MALDI-TOF mass spectra of AHBP and to qualitatively determine the extent of cyclization (side reactions) at each degree of polymerization. Using the adequate set of equations and results obtained from MALDI-TOF mass spectra of AHBP, every signal from the spectra was identified. The obtained results show that formation of poly(bis-MPA), intramolecular esterification and intramolecular etherification occurred as side reactions during the synthesis of these polyesters. The relative amount of the cycles increases with the number of pseudo generation (from the second up to the fifth pseudo generation). It was also observed that the relative proportion of the signals which represent cyclic structures increases with the increasing degree of polymerization. In this work the basic principles of MALDI-TOF MS are also presented, as well as, a review of adequate published articles. PB - Association of Chemical Engineers of Serbia, T2 - Hemijska Industrija T1 - Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom T1 - Characterization of aliphatic hyperbranched polyesters by MALDI-TOF mass spectrometry VL - 61 IS - 6 SP - 333 EP - 341 DO - 10.2298/HEMIND0706333V ER -
@article{ author = "Vuković, Jasna and Jovanović, Slobodan and Lechner, Manfred D.", year = "2007", abstract = "U okviru ovog rada prikazani su rezultati ispitivanja opsega sporednih proizvoda (ciklika) kod hidroksi-funkcionalnih alifatskih hiperrazgranatih poliestara primenom MALDI-TOF masene spektrometrije. Istovremeno su opisani i osnovni principi MALDI-TOF masene spektrometrije i dat je kratak literaturni pregled., In this work, MALDI-TOF mass spectrometry was used for the characterization of aliphatic hyperbranched polyesters (AHBP), synthesized from 2,2-bis(hydroxymethyl)propionic acid (bis-MPA) and di-trimethylolpropane. From the obtained results it was concluded that it was not possible to take complete advantages of MALDI-TOF MS in this particular case, since the AHBP used in this work were polydisperse. The intensity of the signals from the high mass tail of these samples (pseudo generation higher than four) was underestimated and insufficient to distinguish it from the baseline and to use it for the analysis of the spectra. As a consequence of that, lower values of the Mn were obtained. At the same time, Mw were also underestimated, which led to very low values of the polydispersity index. On the other hand, it was possible to obtain molar masses of individual molecules from the MALDI-TOF mass spectra of AHBP and to qualitatively determine the extent of cyclization (side reactions) at each degree of polymerization. Using the adequate set of equations and results obtained from MALDI-TOF mass spectra of AHBP, every signal from the spectra was identified. The obtained results show that formation of poly(bis-MPA), intramolecular esterification and intramolecular etherification occurred as side reactions during the synthesis of these polyesters. The relative amount of the cycles increases with the number of pseudo generation (from the second up to the fifth pseudo generation). It was also observed that the relative proportion of the signals which represent cyclic structures increases with the increasing degree of polymerization. In this work the basic principles of MALDI-TOF MS are also presented, as well as, a review of adequate published articles.", publisher = "Association of Chemical Engineers of Serbia,", journal = "Hemijska Industrija", title = "Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom, Characterization of aliphatic hyperbranched polyesters by MALDI-TOF mass spectrometry", volume = "61", number = "6", pages = "333-341", doi = "10.2298/HEMIND0706333V" }
Vuković, J., Jovanović, S.,& Lechner, M. D.. (2007). Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom. in Hemijska Industrija Association of Chemical Engineers of Serbia,., 61(6), 333-341. https://doi.org/10.2298/HEMIND0706333V
Vuković J, Jovanović S, Lechner MD. Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom. in Hemijska Industrija. 2007;61(6):333-341. doi:10.2298/HEMIND0706333V .
Vuković, Jasna, Jovanović, Slobodan, Lechner, Manfred D., "Karakterizacija alifatskih hiperrazgranatih poliestara MALDI-TOF masenom spektrometrijom" in Hemijska Industrija, 61, no. 6 (2007):333-341, https://doi.org/10.2298/HEMIND0706333V . .