MALDI-TOF MS stability study of model poly(p-phenylene terephthalamide)s |
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Authors: | Anthony P Gies Anton Schotman David M Hercules |
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Institution: | (1) Department of Chemistry, Vanderbilt University, 7330 Stevenson Center, Nashville, TN 37235, USA;(2) Teijin Aramid BV, P. O. Box 9600, 6800 TC Arnhem, Netherlands |
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Abstract: | In the present study, we address the possibility of matrix-assisted laser desorption/ionization (MALDI)–time-of-flight MS
analysis-induced chain fragmentation in poly(p-phenylene terephthalamide) (PPD-T) by considering two possible sources: (1) grinding-induced fragmentation resulting from
the evaporation–grinding MALDI sample preparation method (E-G method) and (2) in-source/metastable fragmentation induced by
the MALDI laser. An analysis of variance (ANOVA) statistical study found, with a high probability, that obtaining MALDI spectra
with the effective laser area as large as possible (the “fanned-out” setting) did not cause any chain fragmentation due to
the E-G MALDI sample preparation method, even when three additional grinding steps were used. However, the effect of laser
fluence was less clear. A significant effect of laser fluence was observed for lower mass oligomers (<1,400 Da), but there
was essentially no effect for higher mass species up to our limit of ANOVA measurement (∼2,300 Da). Plausible explanations
are presented to explain these observations. The most likely scenario is that “unexpected” end-group modifications occur during
PPD-T synthesis, producing small quantities of low mass species, which are amplified by the MALDI-EG extraction procedure. |
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