Structural Characterization of Polymeric Materials by Mass Spectrometry

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  • SATO Hiroaki
    Research Institute for Environmental Management Technology, National Institute of Advanced Industrial Science and Technology (AIST)

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  • 質量分析法を用いたポリマー材料の構造解析
  • シツリョウ ブンセキホウ オ モチイタ ポリマー ザイリョウ ノ コウゾウ カイセキ

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Abstract

The development of new polymer characterization techniques is constantly required to understand the various properties of polymers and create new functional polymers. In this study, two mass spectrometry (MS) approaches have been investigated: temperature programmed pyrolysis-mass spectrometry (TPPy-MS) and soft laser desorption/ionization-mass spectrometry (SLD-MS). The study can be summarized as follows:<br> 1) A TPPy-MS system was developed to overcome the limitations of conventional evolved gas analysis (EGA) systems such as thermogravimetry/MS (TG/MS). The TPPy-MS system was used to investigate the mechanisms of thermal degradation of an engineering polymer with a brominated flame-retardant, and the intermolecular interaction mechanisms of miscible polymer blends and polymer/clay hybrids.<br> 2) Matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS) was employed to characterize the chemical structure of each polymer chain. A new data processing method for size exclusion chromatography (SEC)/MALDI-MS was proposed to determine the accurate molecular weight distribution of polymers based on individual oligomer compositions. MALDI-MS was also used to investigate the biodegradation behavior of polymers. Based on the structural changes in each polymer chain, enzymatic degradation mechanisms of a biodegradable polyester and bacterial degradation of surfactants have been proposed.<br> 3) To avoid the use of matrix reagents that frequently interfere with the mass spectra of oligomer and polymer additives, novel ionization platforms for matrix-free SLD-MS were investigated. The etching conditions of porous silicon spots for desorption/ionization on porous silicon-mass spectrometry (DIOS-MS) were optimized to determine the accurate molecular weight distribution of a certified reference polystyrene. Finally, two ionization platforms were developed using a pyroelectric ceramic plate and germanium nanodot deposited on a silicon wafer. The latter method was preferred for characterization of brominated flame-retardants.

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