0000000000636914
AUTHOR
Ralph-peter Krüger
Quantitative analysis of broad molecular weight distributions obtained by matrix-assisted laser desorption ionisation-time-of-flight mass spectrometry
In order to quantify the error of matrix-assisted laser desorption ionisation (MALDI) time-of-flight (TOF) mass spectrometry in the determination of broad molecular weight distributions, different mixtures by weight of two poly(methyl methacrylate) standards were prepared. These mixtures, with well-defined bimodal molecular weight distributions were analysed by MALDI-TOF mass spectrometry using different matrices (2,4,6-trihydroxyacetophenone and 2,5-dihydroxybenzoic acid) and different cations (Li+, Na+, K+, Rb+ and Cs+) for doping the analyte. From the MALDI-TOF mass spectrometric data, the weight fractions of the two polymers of all mixtures were determined and compared to the values mea…
Mechanism of anionic polymerization of (meth)acrylates in the presence of aluminium alkyls
Summary Methyl methacrylate was polymerized with tert-butyl lithium in the presence of triethylaluminum or triisobutylaluminium at -78~ in toluene. As indicated by GPC and MALDI-TOF mass spectrometry, the polymerization is accompanied by side reactions. The lower oligomers were fractionated by distillation and characterised by NMR, FT-IR, UV and electron impact (EI) mass spectrometry. All these data show that part of the polymer chains are carrying exactly one tert-butyl isoprenyl ketone unit. In order to avoid the formation of tert-butyl isoprenyl ketone a molar ratio of A1/Li > 2 is necessary.