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Related Concept Videos

Metallic Solids02:37

Metallic Solids

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Metallic solids such as crystals of copper, aluminum, and iron are formed by metal atoms. The structure of metallic crystals is often described as a uniform distribution of atomic nuclei within a “sea” of delocalized electrons. The atoms within such a metallic solid are held together by a unique force known as metallic bonding that gives rise to many useful and varied bulk properties.
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Solids in which the atoms, ions, or molecules are arranged in a definite repeating pattern are known as crystalline solids. Metals and ionic compounds typically form ordered, crystalline solids. A crystalline solid has a precise melting temperature because each atom or molecule of the same type is held in place with the same forces or energy. Amorphous solids or non-crystalline solids (or, sometimes, glasses) which lack an ordered internal structure and are randomly arranged. Substances that...
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Network covalent solids contain a three-dimensional network of covalently bonded atoms as found in the crystal structures of nonmetals like diamond, graphite, silicon, and some covalent compounds, such as silicon dioxide (sand) and silicon carbide (carborundum, the abrasive on sandpaper). Many minerals have networks of covalent bonds.
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Molecular and Ionic Solids02:54

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Crystalline solids are divided into four types: molecular, ionic, metallic, and covalent network based on the type of constituent units and their interparticle interactions.
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¹³C NMR: ¹H–¹³C Decoupling01:04

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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
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Particles in a solid are tightly packed together (fixed shape) and often arranged in a regular pattern; in a liquid, they are close together with no regular arrangement (no fixed shape); in a gas, they are far apart with no regular arrangement (no fixed shape). Particles in a solid vibrate about fixed positions (cannot flow) and do not generally move in relation to one another; in a liquid, they move past each other (can flow) but remain in essentially constant contact; in a gas, they move...
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Refocused linewidths less than 10 Hz in 1H solid-state NMR.

Federico M Paruzzo1, Gabriele Stevanato1, Meghan E Halse2

  • 1Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), Lausanne 1015, Switzerland.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|June 12, 2018
PubMed
Summary

Researchers found an oscillation limiting proton (¹H) coherence lifetimes in solid-state NMR. A double spin-echo technique removes this, extending lifetimes significantly for improved spectral resolution.

Keywords:
Coherence lifetimeHigh-resolutionHomonuclear dipolar decouplingSolid-state NMRT(2)′ measurements

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Quantum Coherence Phenomena
  • Materials Science

Background:

  • Proton (¹H) coherence lifetimes in homonuclear dipolar decoupled solid-state NMR experiments are typically limited to a few milliseconds.
  • This limited coherence time restricts spectral resolution and the ability to probe complex molecular dynamics in solid materials.
  • Understanding and overcoming these limitations is crucial for advancing NMR applications in chemistry, biology, and materials science.

Purpose of the Study:

  • To identify the underlying cause of the limited coherence lifetimes observed in ¹H solid-state NMR experiments.
  • To develop and validate a method to extend coherence lifetimes beyond the typical few milliseconds.
  • To demonstrate the practical benefits of extended coherence lifetimes, such as improved spectral resolution.

Main Methods:

  • Acquisition and analysis of spin-echo dephasing curves in homonuclear dipolar decoupled ¹H solid-state NMR.
  • Implementation and application of a double spin-echo pulse sequence.
  • Characterization of coherence lifetimes and refocused linewidths in model compounds (adamantane and β-AspAla).

Main Results:

  • Discovery of an oscillation in spin-echo dephasing curves, identified as a limiting factor for coherence lifetimes.
  • Successful removal of the coherence-limiting oscillation using a double spin-echo experiment.
  • Achieved significantly extended coherence lifetimes: >45 ms in adamantane and >22 ms in β-AspAla.
  • Resulting refocused linewidths were reduced to <7 Hz in adamantane and <14 Hz in β-AspAla.

Conclusions:

  • The observed oscillation is a key factor limiting coherence lifetimes in standard ¹H solid-state NMR experiments.
  • The double spin-echo technique effectively suppresses this oscillation, enabling substantially longer coherence lifetimes.
  • Extended coherence lifetimes lead to dramatic improvements in spectral resolution, enhancing the utility of solid-state NMR.