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Related Concept Videos

Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
¹H NMR Chemical Shift Equivalence: Homotopic and Heterotopic Protons01:03

¹H NMR Chemical Shift Equivalence: Homotopic and Heterotopic Protons

Protons in identical electronic environments within a molecule are chemically equivalent and have the same chemical shift. The replacement test is a useful tool to identify chemical equivalence and predict NMR spectra. A substituent replaces each of the protons being examined and the resulting molecules are compared. If the same molecule is obtained, the protons are equivalent or homotopic. Replacement of any hydrogens in ethane by chlorine yields chloroethane because all six protons are...
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

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 axis.

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Updated: Jul 7, 2026

Rapid Mix Preparation of Bioinspired Nanoscale Hydroxyapatite for Biomedical Applications
05:41

Rapid Mix Preparation of Bioinspired Nanoscale Hydroxyapatite for Biomedical Applications

Published on: February 23, 2017

Revisiting silicate substituted hydroxyapatite by solid-state NMR.

G Gasquères1, C Bonhomme, J Maquet

  • 1Université Pierre et Marie Curie-Paris6, UMR 7574 CNRS, Laboratoire de Chimie de la Matière Condensée de Paris, Paris, F-75005, France.

Magnetic Resonance in Chemistry : MRC
|February 29, 2008
PubMed
Summary
This summary is machine-generated.

Silicon-substituted hydroxyapatite (Si-HAp) shows potential for bone implants. Solid-state NMR reveals that silicon incorporation into the HAp structure is limited, with much forming external silica-gel units.

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Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry
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Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

Published on: October 18, 2019

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Rapid Mix Preparation of Bioinspired Nanoscale Hydroxyapatite for Biomedical Applications
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Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry
09:37

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

Published on: October 18, 2019

Area of Science:

  • Biomaterials Science
  • Materials Chemistry
  • Solid-State Chemistry

Background:

  • Silicon-substituted hydroxyapatite (Si-HAp) exhibits enhanced bone remodeling properties, making it a promising material for biomedical implants.
  • Previous structural characterization of Si-HAp primarily relied on indirect methods like X-ray and neutron diffraction.

Purpose of the Study:

  • To precisely determine the structural location of silicon within Si-HAp synthesized via precipitation.
  • To differentiate between silicon incorporated into the hydroxyapatite lattice and silicon present as separate silica phases.

Main Methods:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy was employed for detailed structural analysis.
  • Specific NMR techniques included (29)Si Magic Angle Spinning (MAS), (1)H -->(29)Si Cross-Polarization MAS (CP MAS), and T(1)rho((1)H) edited (1)H -->(29)Si CP MAS experiments.

Main Results:

  • Solid-state NMR demonstrated that in 4.6 wt% Si-HAp, only a fraction of silicon atoms are incorporated into the hydroxyapatite (HAp) lattice as Q(0) (SiO(4) (4-)) species.
  • A significant portion of the silicate units were identified as silica-gel species located outside the HAp structure.
  • The T(1)rho((1)H) edited sequence proved crucial for unambiguously distinguishing the location of SiO(4) (4-) moieties.

Conclusions:

  • Precipitation methods yield Si-HAp where silicon incorporation into the HAp lattice is limited.
  • The presence of external silica-gel units alongside lattice-incorporated silicon impacts the material's properties.
  • Solid-state NMR, particularly with advanced editing sequences, provides definitive insights into the structural state of silicon in Si-HAp.