Analysis of the End Groups in Derivatized Poly(lactic acid) and the Junction Unit in Chain-extended Poly(lactic acid) by DOSY

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  • SOGABE Keisuke
    Department of Chemical Science and Technology, The University of Tokushima Kaneka Techno Research Co., Ltd.
  • UTE Koichi
    Department of Chemical Science and Technology, The University of Tokushima

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Other Title
  • 誘導体化ポリ乳酸の末端基及び鎖延長したポリ乳酸の接合部位のDOSYによる分析
  • ユウドウタイカ ポリ ニュウサン ノ マッタンキ オヨビ クサリエンチョウ シタ ポリ ニュウサン ノ セツゴウ ブイ ノ DOSY ニ ヨル ブンセキ

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Abstract

The hydroxyl and carboxyl end-groups in poly(lactic acid) (PLA) were derivatized with trimethylsilylation or trifluoroacetylation to be detected by 1H DOSY or 19F DOSY with enhanced sensitivity. The diffusion coefficients (D) for the derivatized end-groups of PLA in a chloroform-d solution were determined by 1H and 19F DOSY analysis; the values agreed well with each other. The D values for the end groups were found to be larger than those for the methyl and methine groups in repeating units of the PLA. The relative intensity of the 1H DOSY resonances due to the trimethylsilyl end-group and the main-chain methyl group allowed us to evaluate the dependence of the degree of polymerization on D. 1H DOSY analysis of PLA treated with diphenylmethane diisocyanate (MDI) was also carried out to determine D for the junction unit in the PLA. The result clearly indicated that the molecular weight of the PLA increased by the reaction of MDI and the hydroxyl end-groups.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 63 (2), 93-99, 2014

    The Japan Society for Analytical Chemistry

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