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Related Concept Videos

¹H NMR of Labile Protons: Deuterium (²H) Substitution00:48

¹H NMR of Labile Protons: Deuterium (²H) Substitution

1.2K
This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is the use of deuterium. Amongst the three isotopes of hydrogen, deuterium (2H) has a nucleus composed of one proton and one neutron. When the D2O solvent is added to a pure dry ethanol solution, its labile proton is substituted with deuterium.
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¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)

1.4K
When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
1.4K
Proton (¹H) NMR: Chemical Shift01:07

Proton (¹H) NMR: Chemical Shift

3.0K
Organic molecules primarily contain carbon and hydrogen atoms. While all the hydrogen isotopes are NMR-active, protium or hydrogen-1 is the most abundant. It has a significant energy separation between its nuclear spin states due to its large gyromagnetic ratio. As per Boltzmann's distribution, an increase in the energy separation implies a greater excess population of nuclei available for excitation, resulting in a strong NMR absorption signal.
Absorption signals of all the protium nuclei...
3.0K
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

1.2K
Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
1.2K
¹H NMR of Labile Protons: Temporal Resolution01:10

¹H NMR of Labile Protons: Temporal Resolution

1.5K
Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
The –OH proton in alcohols typically appears in the range of δ 2 to 5 ppm but can vary depending on the specific...
1.5K
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

597
Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other...
597

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Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis
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Characterization of hydrogenated dentin components by advanced 1H solid-state NMR experiments.

Yannick Coppel1, Yann Prigent2, Geneviève Grégoire3

  • 1Laboratoire de Chimie de Coordination UPR8241, CNRS, 205 Rte de Narbonne, F-31077, Toulouse Cedex 04, France.

Acta Biomaterialia
|August 30, 2020
PubMed
Summary

This study introduces novel solid-state Nuclear Magnetic Resonance (ssNMR) experiments for detailed molecular analysis of human dentin. These methods enhance understanding of biomaterial structure and mechanical properties by characterizing hydrogen-containing species.

Keywords:
(1)H MAS NMRApatitic biomaterialChemical organisationDentin compositionSolid state NMRWater molecules

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Area of Science:

  • Biomaterials Science
  • Biophysics
  • Solid-State Chemistry

Background:

  • Understanding the molecular organization of biological materials like bone and dentin is crucial for elucidating their mechanical properties.
  • Solid-state Nuclear Magnetic Resonance (ssNMR) offers atomic-level structural insights into amorphous composite materials.
  • 1H magic angle spinning (MAS) ssNMR, while useful, faces challenges in resolving overlapping signals from species like water and hydroxyl groups.

Purpose of the Study:

  • To develop and present a set of ssNMR experiments for the detailed 1H characterization of human dentin components.
  • To improve the identification and localization of hydrogen-containing species within dentin's complex matrix.
  • To provide a tool for understanding structural and dynamic information relevant to biomaterial modifications.

Main Methods:

  • Utilized a series of ssNMR experiments focusing on homo- and hetero-nuclear dipolar couplings, primarily fast 1D experiments.
  • Employed straightforward sample modifications including vacuum drying, deuterium exchange, and demineralization to aid 1H assignment.
  • Applied these methods to distinguish signals from water molecules, HPO42-, and OH- groups based on their location and dynamics.

Main Results:

  • Successfully assigned 1H signals for key dentin species, differentiating their roles and environments.
  • Demonstrated the ability to identify water molecules, phosphate, and hydroxyl groups based on their localization (organic phase, apatite-bound, interface) and mobility.
  • Validated a new ssNMR 'toolbox' for analyzing the structural and dynamic characteristics of biomaterials.

Conclusions:

  • The proposed ssNMR methodology effectively characterizes 1H signals in human dentin, overcoming resolution limitations.
  • This approach provides critical structural and dynamic information on biomaterial components, particularly water molecules.
  • The ssNMR toolbox holds significant potential for advancing the study of chemical and physical modifications in apatitic biomaterials.