High resolution 1H spectra of powdered solids observed by Hahn echo pulse sequence with magic-angle spinning

Jian Zhi Hu, Jinyuan Zhou, Feng Deng, Hanqiao Feng, Nianhua Yang, Liyun Li, Chaohui Ye

Research output: Contribution to journalArticle

Abstract

The 1H magic-angle spinning (MAS) spectrum for a typical powdered solid is composed of a high resolution component and a broadline component. The high resolution component can be well isolated from the broadline component by the Hahn echo sequence with a long echo time. Compared with the CRAMPS experiment, which measures the proton system as a whole, the high resolution echo-MAS method measures only a fraction of the solid, which is usually small at room temperature and quite different from the majority of the solid in both molecular motion and chemical environment. It is shown that for a sample of fumaric acid monoethyl ester, the chemical shifts of the high resolution component are apparently distinguishable from the isotropic chemical shifts of the broadline component in the CRAMPS spectrum as the temperature approaches the melting point. In addition, for a sample of malonic acid, the echo-MAS spectrum is sensitive to moisture and temperature, while its corresponding CRAMPS spectrum is not. It is suggested that the molecules which produce the high resolution component are related to the lattice defects in a solid, including the surface disorder of the polycrystallites, while the molecules that generate the broadline component are located on the rigid lattice of the solid.

Original languageEnglish (US)
Pages (from-to)85-94
Number of pages10
JournalSolid State Nuclear Magnetic Resonance
Volume6
Issue number1
DOIs
StatePublished - Feb 1996
Externally publishedYes

Fingerprint

Magic angle spinning
metal spinning
echoes
high resolution
pulses
Chemical shift
Molecules
Acids
Crystal defects
chemical equilibrium
Temperature
Melting point
Protons
Esters
Moisture
acids
moisture
melting points
esters
molecules

Keywords

  • CRAMPS
  • Delayed acquisition
  • Hahn echo
  • High resolution H spectrum
  • Magic-angle spinning

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Spectroscopy
  • Electronic, Optical and Magnetic Materials

Cite this

High resolution 1H spectra of powdered solids observed by Hahn echo pulse sequence with magic-angle spinning. / Hu, Jian Zhi; Zhou, Jinyuan; Deng, Feng; Feng, Hanqiao; Yang, Nianhua; Li, Liyun; Ye, Chaohui.

In: Solid State Nuclear Magnetic Resonance, Vol. 6, No. 1, 02.1996, p. 85-94.

Research output: Contribution to journalArticle

Hu, Jian Zhi ; Zhou, Jinyuan ; Deng, Feng ; Feng, Hanqiao ; Yang, Nianhua ; Li, Liyun ; Ye, Chaohui. / High resolution 1H spectra of powdered solids observed by Hahn echo pulse sequence with magic-angle spinning. In: Solid State Nuclear Magnetic Resonance. 1996 ; Vol. 6, No. 1. pp. 85-94.
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AB - The 1H magic-angle spinning (MAS) spectrum for a typical powdered solid is composed of a high resolution component and a broadline component. The high resolution component can be well isolated from the broadline component by the Hahn echo sequence with a long echo time. Compared with the CRAMPS experiment, which measures the proton system as a whole, the high resolution echo-MAS method measures only a fraction of the solid, which is usually small at room temperature and quite different from the majority of the solid in both molecular motion and chemical environment. It is shown that for a sample of fumaric acid monoethyl ester, the chemical shifts of the high resolution component are apparently distinguishable from the isotropic chemical shifts of the broadline component in the CRAMPS spectrum as the temperature approaches the melting point. In addition, for a sample of malonic acid, the echo-MAS spectrum is sensitive to moisture and temperature, while its corresponding CRAMPS spectrum is not. It is suggested that the molecules which produce the high resolution component are related to the lattice defects in a solid, including the surface disorder of the polycrystallites, while the molecules that generate the broadline component are located on the rigid lattice of the solid.

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