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Structural analysis of cross-linking structures in rubbers by zero-field solid-state 33S NMR

Research Project

Project/Area Number 21K05129
Research Category

Grant-in-Aid for Scientific Research (C)

Allocation TypeMulti-year Fund
Section一般
Review Section Basic Section 34020:Analytical chemistry-related
Research InstitutionKochi University

Principal Investigator

Yamada Kazuhiko  高知大学, 教育研究部総合科学系複合領域科学部門, 准教授 (80373380)

Project Period (FY) 2021-04-01 – 2024-03-31
Project Status Completed (Fiscal Year 2023)
Budget Amount *help
¥4,290,000 (Direct Cost: ¥3,300,000、Indirect Cost: ¥990,000)
Fiscal Year 2023: ¥1,300,000 (Direct Cost: ¥1,000,000、Indirect Cost: ¥300,000)
Fiscal Year 2022: ¥1,690,000 (Direct Cost: ¥1,300,000、Indirect Cost: ¥390,000)
Fiscal Year 2021: ¥1,300,000 (Direct Cost: ¥1,000,000、Indirect Cost: ¥300,000)
Keywords加硫ゴム / 硫黄 / 無磁場固体NMR / NMR / 架橋構造 / シスチン / ゴム / 固体NMR
Outline of Research at the Start

1830年代に加硫ゴムが発見されて以来、ゴムは現在社会に欠かすことの出来ないマテリアルである。しかしながら、ゴムのマクロ物性を決定づける硫黄原子による架橋構造は未だに明らかになっていない。本研究の目的は、アモルファス試料においても硫黄原子の化学分析が可能な、超高感度化無磁場固体核磁気共鳴(NMR)法を開発し、世界初となる、ゴム中の硫黄原子を介した架橋構造を分子レベルで解明することである。

Outline of Final Research Achievements

Since the discovery of vulcanized rubber in the 1830s, the range of rubber applications has expanded dramatically, including automotive tires. However, the cross-linking structure of rubber by sulfur atoms, which determines the macro physical properties of rubber, has not yet been clarified. The reason for this is that there has been no suitable analysis method to observe and analyze sulfur atoms in amorphous samples. In this study, we have developed a new methodology based on zero-magnetic field sulfur-33 nuclear magnetic resonance that enables local structure analysis of sulfur atoms even in amorphous samples including vulcanized rubber.

Academic Significance and Societal Importance of the Research Achievements

加硫ゴムの硫黄原子による架橋構造は長年に渡り明らかになっていなかった。本研究で開発した無磁場固体硫黄NMR法を活用することで、アモルファス試料における硫黄原子の定性・定量解析が可能になる。エラストマー研究において、革新的な分析手法を提供することができる。

Report

(3 results)
  • 2023 Final Research Report ( PDF )
  • 2022 Research-status Report
  • 2021 Research-status Report
  • Research Products

    (5 results)

All 2023 2022

All Journal Article (4 results) (of which Int'l Joint Research: 3 results,  Peer Reviewed: 3 results) Presentation (1 results)

  • [Journal Article] A sulfur-33 Nuclear Quadrupole Resonance Study of 33S2-labeled L-Cystine2023

    • Author(s)
      K. Yamada*, Y. Masuda
    • Journal Title

      Magn. Reson. Chem

      Volume: 61 Pages: 296-300

    • Related Report
      2022 Research-status Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Field-Stepwise-Swept Solid-State 35Cl NMR and NQR of trichloroisocyanuric acid2023

    • Author(s)
      K. Yamada*, M. Takahashi, T. Tritrakarn, T. Okamur
    • Journal Title

      Chem. Phys. Lett.

      Volume: 811

    • Related Report
      2022 Research-status Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] 有機硫黄化合物を測定対象とする無磁場固体核磁気共鳴(NMR)法の応用2022

    • Author(s)
      山田 和彦
    • Journal Title

      生物物理

      Volume: 62 Pages: 242-245

    • Related Report
      2022 Research-status Report
  • [Journal Article] Multinuclear Solid-state Nuclear Magnetic Resonance of coal2022

    • Author(s)
      K. Yamada
    • Journal Title

      ISIJ International

      Volume: 62 Pages: 840-848

    • Related Report
      2021 Research-status Report
    • Peer Reviewed / Int'l Joint Research
  • [Presentation] 次世代型固体NMR法を活用した石炭化学構造研究2022

    • Author(s)
      山田 和彦
    • Organizer
      日本鉄鋼協会第184回秋季講演大会,
    • Related Report
      2022 Research-status Report

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Published: 2021-04-28   Modified: 2025-01-30  

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