Determination of molecular mass distribution of silicone oils
by supercritical fluid chromatography, matrix-assisted laser
desorption ionization time-of-flight mass spectrometry and
their off-line combination

J 2001

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination

CHMELÍK, Josef, Josef PLANETA, Pavel ŘEHULKA a Josef CHMELÍK

Základní údaje

Originální název

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination

Autoři

CHMELÍK, Josef, Josef PLANETA, Pavel ŘEHULKA a Josef CHMELÍK

Vydání

Journal of Mass Spectrometry, John Wiley & Sons, Ltd. 2001, 1076-5174

Další údaje

Typ výsledku

Článek v odborném periodiku

Utajení

není předmětem státního či obchodního tajemství

Impakt faktor

Impact factor: 2.685

Organizační jednotka

Přírodovědecká fakulta

UT WoS

000170299700007

Klíčová slova anglicky

gel-permeation chromatography; MALDI-TOF; synthetic-polymers; polydispersity; fractionation; performance

Štítky

fractionation, gel-permeation chromatography, MALDI-TOF, performance, polydispersity, synthetic-polymers

Příznaky

Mezinárodní význam, Recenzováno

Změněno: 10. 1. 2007 19:26, Mgr. Josef Chmelík, Ph.D.

Anotace

V originále

Silicone oil samples were characterized by supercritical fluid chromatography (SFC), matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS), and their off-line combination. SFC was used to separate samples of silicone oils on micropacked capillary columns. The fractions for the identification studies were obtained from SFC runs at defined time intervals, when the restrictor was pulled out from the chromatographic flame ionization detector (FID) and inserted into a glass vial with acetone. MALDI-TOF MS was used for the identification of individual oligomers in the fractions separated. The molecular mass distributions determined based on SFC and MALDI-TOF MS measurements were compared. From this comparison, it follows that the results are in good agreement. However, certain differences were observed: MALDI-TOF MS was capable of detecting somewhat larger oligomers than the SFC-FID, but the lower molecular mass oligomers were not present in the MALDI spectra. Differences in the region of lower molecular masses can be explained by evaporation of the more volatile low molecular mass oligomers resulting from heating of the sample during the MALDI-TOF MS measurements as a result of the absorption of the laser shot energy. The fact that no high mass discrimination effects of the MALDI-TOF MS measurements, compared with SFC, were observed is very promising for further applications of MALDI-TOF MS in characterizing synthetic polymers of moderate polydispersity.

Citovat

CHMELÍK, Josef, Josef PLANETA, Pavel ŘEHULKA a Josef CHMELÍK. Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination. Journal of Mass Spectrometry. John Wiley & Sons, Ltd., 2001, roč. 36, č. 7, s. 760-770, 10 s. ISSN 1076-5174.

@article{708498,
   author = {Chmelík, Josef and Planeta, Josef and Řehulka, Pavel and Chmelík, Josef},
   article_number = {7},
   keywords = {gel-permeation chromatography; MALDI-TOF; synthetic-polymers; polydispersity; fractionation; performance},
   issn = {1076-5174},
   journal = {Journal of Mass Spectrometry},
   title = {Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination},
   volume = {36},
   year = {2001}
}

TY  - JOUR
ID  - 708498
AU  - Chmelík, Josef - Planeta, Josef - Řehulka, Pavel - Chmelík, Josef
PY  - 2001
TI  - Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination
JF  - Journal of Mass Spectrometry
VL  - 36
IS  - 7
SP  - 760-770
EP  - 760-770
PB  - John Wiley & Sons, Ltd.
SN  - 10765174
KW  - gel-permeation chromatography
KW  - MALDI-TOF
KW  - synthetic-polymers
KW  - polydispersity
KW  - fractionation
KW  - performance
N2  - Silicone oil samples were characterized by supercritical fluid chromatography (SFC), matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS), and their off-line combination. SFC was used to separate samples of silicone oils on micropacked capillary columns. The fractions for the identification studies were obtained from SFC runs at defined time intervals, when the restrictor was pulled out from the chromatographic flame ionization detector (FID) and inserted into a glass vial with acetone. MALDI-TOF MS was used for the identification of individual oligomers in the fractions separated. The molecular mass distributions determined based on SFC and MALDI-TOF MS measurements were compared. From this comparison, it follows that the results are in good agreement. However, certain differences were observed: MALDI-TOF MS was capable of detecting somewhat larger oligomers than the SFC-FID, but the lower molecular mass oligomers were not present in the MALDI spectra. Differences in the region of lower molecular masses can be explained by evaporation of the more volatile low molecular mass oligomers resulting from heating of the sample during the MALDI-TOF MS measurements as a result of the absorption of the laser shot energy. The fact that no high mass discrimination effects of the MALDI-TOF MS measurements, compared with SFC, were observed is very promising for further applications of MALDI-TOF MS in characterizing synthetic polymers of moderate polydispersity.
ER  -

CHMELÍK, Josef, Josef PLANETA, Pavel ŘEHULKA a Josef CHMELÍK. Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix-assisted laser desorption ionization time-of-flight mass spectrometry and their off-line combination. \textit{Journal of Mass Spectrometry}. John Wiley \&{} Sons, Ltd., 2001, roč.~36, č.~7, s.~760-770, 10 s. ISSN~1076-5174.

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