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Development of High-Resolution NMR of Quadrupolar Nuclei and Trial Construction of the Spectrometer

Research Project

Project/Area Number 03504002
Research Category

Grant-in-Aid for Developmental Scientific Research (A)

Allocation TypeSingle-year Grants
Research Field 物理化学一般
Research InstitutionKOYOTO UNIVERSITY

Principal Investigator

TERAO Takehiko  Kyoto Univ., Science, Professor, 理学部, 教授 (50093274)

Co-Investigator(Kenkyū-buntansha) FUJITO Teruaki  Analytical Research Manager Instruments, & Development, 分析機器技術本部, 課長
YOSHIMURA Kazuyoshi  Kyoto Univ., Science, Associate Professor, 理学部, 助教授 (70191640)
KUBO Atushi  Kyoto Univ., Science, Instructor, 理学部, 助手 (20205115)
竹腰 清乃理  京都大学, 理学部, 助教授 (10206964)
Project Period (FY) 1991 – 1993
Project Status Completed (Fiscal Year 1993)
Budget Amount *help
¥41,500,000 (Direct Cost: ¥41,500,000)
Fiscal Year 1993: ¥2,700,000 (Direct Cost: ¥2,700,000)
Fiscal Year 1992: ¥8,000,000 (Direct Cost: ¥8,000,000)
Fiscal Year 1991: ¥30,800,000 (Direct Cost: ¥30,800,000)
Keywordsquadrupolar nuclei / high-resolution solid-state NMR / DAS-NMR / 試料高速回転
Research Abstract

1. A DAS-NMR-system was developed.
2. A computer program for the pulse sequence of DAS-NMR, control of a motor system, and data manipulation, and also a simulation program of one-and two-dimensional spectra were developed to obtain and analyze experimental spectra.
3. It was confirmed by carrying out DAS-NMR for ^<23>Na in Rochelle salt that the NMR system normally works. A resolution of 120 Hz was obtained by using proton decoupling.
4. A simple and sensitive DAS-NMR method was developed which allows us to observe pure-absorption two-dimensional spectra.
5. A new high-resolution NMR spectroscopy of quadrupolar nuclei was proposed which uses ultrasonic sound for dispersing powder in liquid and violently disturbing the particles, It was confirmed from a ^1H NMR study that linewidths become narrower by mixing glass particles.
6. A method by which two-dimensional powder spectra for quadrupolar nuclei can be observed between two different spinning orientations was developed, and successfully applied to ^<27>Al of Rochelle salt.
7. Details of static and dynamic behaviors of the guest molecules in beta-cyclodextrin/ferrocene and cholic acid/gamma-valerolactone inclusion compounds were studied by measuring temperature dependence of ^<13>C chemical shift powder patterns of the guest molecules using SASS spectroscopy.

Report

(4 results)
  • 1993 Annual Research Report   Final Research Report Summary
  • 1992 Annual Research Report
  • 1991 Annual Research Report
  • Research Products

    (36 results)

All Other

All Publications (36 results)

  • [Publications] F.Imashiro: "Study of the Dynamics of Ferrocene Enclathrated in β- and γ-Cyclodextrins by One-Dimensional Switching-Angle Sample Spinning NMR Spectroscopy" Magn.Reson.Chem.30. 796-797 (1992)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] T.Nakai: "Measurements of Heteronuclear Dipolar Powder Patterns Due Only to Directly Bonded Couplings" Magn.Reson.Chem.30. 42-44 (1992)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] D.Kuwahara: "Dynamics of Ferrocene Molecules Enclathrated in β-Cyclodextrin as Studied by Variable-Temperature on-Dimensional SASS NMR" Chem.Phys.Lett.204. 533-537 (1993)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] F.Imashiro: "^<13>C Solid-State NMR Study on Populations,Conformations,and Molecular Motions of γ-Valerolactone Enantiomers" J.Chem.Soc.Perkin Trans.1759-1763 (1993)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] K.Yoshimura: "Copper NQR Study of the La214 System from an Aspect of Microscopic Environment of Copper" Hyperfine Interactions. 79. 867-872 (1993)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] K.Takegoshi: "Determination of the ^<14>N Quadrupole Coupling Tensor of an L-Alanine Single Crystal by Overtone NMR" Chem.Phys.Lett.206. 450-454 (1993)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] 寺尾武彦ら: "実験化学講座5 NMR" 丸善(株), 445 (1991)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] T.Terao: "Encyclopedia of Nuclear Magnetic Resonance" John.Wiley & Sons.Ltd.(in press),

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] F.Imashiro, D.Kuwahara, N.Kitazaki and T.Terao: "Study of the Dynamics of Ferrocene Enclathrated in beta-and gamma-Cyclodextrins by One-Dimensional Switching-Angle Sample Spinning NMR Spectroscopy." Magn. Reson. Chem.30. 796-797 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] T.Nakai and T.Terao: "Measurements of Heteronuclear Dipolar Power Patterns Due Only to Directly Bonded Couplings." Magn. Reson. Chem.30. 42-44 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] D,Kuwahara, F.Imashiro and T.Terao: "Dynamics of Ferrocene Molecules Enclathrated in beta-Cyclodextrin ad Studied by Variable-Temperature One-Dimensional SASS (Switching-Angle Sample Spinning) NMR Spectroscopy." Chem. Phys. Lett.204. 533-537 (1993)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] F.Imashiro, D.Kuwahara and T.Terao: "^<13>C Solid-state NMR Study on Populations, Conformations. and Molecular Motions of gamma-Valerolactone Enclathrated in the Chiral Cholic acid Host." J.Chem. Soc. Perkin Trans.2. 1759-1763 (1993)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] K.Yoshimura, T.Uemura, M.Kato, K.Kusuge, T.Imai and H.Yasuoka: "Copper NQR Study of La214 System from an Aspect of Microscopic Environment of Copper." Hyp. Int.79. 867-872 (1993)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] K.Takegoshi and K.Hikichi: "Determination of the ^<14>N Quadrupole Coupling Tensor of an L-Alanine Single Crystal by Overtone NMR." Chem. Phys. Lett.206. 450-454 (1993)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] T.Terao et al.: Jikken Kagaku Koza 5, NMR.Maruzen Ltd., 445 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] T,Terao: Encyclopedia of Nuclear Magnetic Resonance (inpress). John. Wiley & Sons. Ltd.,

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1993 Final Research Report Summary
  • [Publications] D.Kuwahara: "Dynamics of ferrocene molecules enclathrated in β-cyclodextrin as studied by variable-temperature on-dimensional SASS NMR" Chem.Phys.Lett.204. 533-537 (1993)

    • Related Report
      1993 Annual Research Report
  • [Publications] F.Imashiro: "13C Solid-State NMR Study on Populations,Conformations,and Molecular Motions of γ-Valerolactone Enantiomers" J.Chem.Soc.Perkin Trans.1759-1763 (1993)

    • Related Report
      1993 Annual Research Report
  • [Publications] A.Kubo: "Proton Two-Dimentional Exchange Naclear Magnetic Resonance Study of a P-Xylene-d_6 Zeolite Inclusion Compound" Mol.Phys.(in press).

    • Related Report
      1993 Annual Research Report
  • [Publications] K.Yoshimura: "Compositional Phase Separation in La_<2-x>Ba_xCuO_y near the Optimum Composition for Superconductivity" J.Phys.Soc.Jpn.62. 1114-1117 (1993)

    • Related Report
      1993 Annual Research Report
  • [Publications] K.Yoshimura: "Copper NQR Study of the La214 System from an Aspect of Microscopic Environment of Copper" Hyperfine Interactions. 79. 867-872 (1993)

    • Related Report
      1993 Annual Research Report
  • [Publications] K.Takegoshi: "Determination of the ^<14>N Quadrupole Coupling Tensor of an L-Alanine Single Crystal by Overtone NMR" Chem.Phys.Lett.206. 450-454 (1993)

    • Related Report
      1993 Annual Research Report
  • [Publications] T.Terao: "Encyclopedia of Nuclear Magnetic Resonance" John.Wiley & Sons.Ltd.(in press),

    • Related Report
      1993 Annual Research Report
  • [Publications] F.Imashiro: "Study of the Dynamics of Ferrocene Enclathrated in β-and γ-cyclodextrins by One-Dimensional Swicning-Angle Sample Spinning NMR Spectroscopy" Magn.Reson.Chem.30. 796-797 (1992)

    • Related Report
      1992 Annual Research Report
  • [Publications] T.Nakai: "Measurements of Heteronuclear Dipolar Powder Pattterns Dve Only to Directly Bonded Couplings" Magn.Reson.Chem.30. 42-44 (1992)

    • Related Report
      1992 Annual Research Report
  • [Publications] A.Kubo: " ^<13>C-Detected ^1H Dipolar Magic-Angle-Spinning NMR Experiments with Isotropic Mixing" J.Magn.Reson.100. 517-537 (1992)

    • Related Report
      1992 Annual Research Report
  • [Publications] K.Yoshimura: "Magnetic Phase Differentiation in the Laz-x Srx CuOy Systems-Cu and La Nuclear Quadrupole Resonance and Relaxation-" Springer Proceedengs in Physics. 60. 405-407 (1992)

    • Related Report
      1992 Annual Research Report
  • [Publications] K.Yoshimura: "Copper NQR Study of the Laz_<14> Sytem from an Aspect of Microscopic Environment of Copper" Hyp.Int.

    • Related Report
      1992 Annual Research Report
  • [Publications] D.Kuwahara: "Dynamics of Ferrocene Molecules Enclathrated in β-Cyclodextrin as studied by Variable-Temperature One-Dimensional SASS(Switching-Angle Somple Spinning)NMR Spectroscopy" Chem.Phys.Lett.

    • Related Report
      1992 Annual Research Report
  • [Publications] Toshihito Nakai,Takehiko Terao: "Measurements of Heteronuclear Dipolar Powder Patterns Due Only to Directly Bonded Couplings" Magn.Reson.Chem.30. 42-44 (1992)

    • Related Report
      1991 Annual Research Report
  • [Publications] F.Imashiro,N.Kitazaki,D.Kuwahara,T.Nakai,T.Terao: "Dynamics of Ferrocene Enclathrated in Deoxycholic Acid as Studied by SASS (Switching-angle Sample Spinning) NMR Spectroscopy" J.Chem.Soc.,Chem.Commun.2. 85-86 (1991)

    • Related Report
      1991 Annual Research Report
  • [Publications] 寺尾 武彦: "固体二次元NMR" 応用物理. 60. 1035-1036 (1991)

    • Related Report
      1991 Annual Research Report
  • [Publications] T.Terao: "Solid-state NMR in Japan" trends in analytical chemistry. 10. 222-225 (1991)

    • Related Report
      1991 Annual Research Report
  • [Publications] F.Imashiro,D.Kuwahara,T.Terao: "Conformational Inequivalence of γ-Valerolactone Enantiomers Enclathrated in Cholic Acid as Elucidated by one-dimensional SASS (Switching-Angle Sample Spinning) NMR Spectroscopy"

    • Related Report
      1991 Annual Research Report
  • [Publications] T.Uegaki,T.Terao: "Simple and high-sensitive pure-absorption-phase dynamic-angle spinning."

    • Related Report
      1991 Annual Research Report
  • [Publications] 寺尾 武彦ら19名: "実験化学講座5 NMR" 丸善(株), 445 (1991)

    • Related Report
      1991 Annual Research Report

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Published: 1991-04-01   Modified: 2016-04-21  

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