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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...
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...
Mass Spectrum: Interpretation01:24

Mass Spectrum: Interpretation

An unknown compound can be established by identifying the molecular ion peak in the mass spectrum. The molecular ion peak is often weak or absent due to the predominance of fragmentation in high-energy electron beams. In such cases, a soft-energy electron beam can be used to scan the spectrum to enhance the intensity of the molecular ion peak. Additionally, chemical ionization, field ionization, and desorption ionization spectra are used to obtain a relatively intense molecular ion peak.To...
High-Resolution Mass Spectrometry (HRMS)01:15

High-Resolution Mass Spectrometry (HRMS)

The resolution of a mass spectrometer depends on the efficiency of separating ions with different ion masses. The mass of an atom is approximated to the sum of the masses of protons and neutrons inside, considering the masses of protons and neutrons as equal. However, the masses of the proton (1.6726 × 10−24 g) and neutron (1.6749 × 10−24 g) are not truly equal. There is a minor error in the expression of atomic masses relative to the simplest atom of hydrogen. For example, the mass of helium...
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...
Polymers: Molecular Weight Distribution01:10

Polymers: Molecular Weight Distribution

For any given polymer, the weight average molecular weight (Mw) is higher than, if not equal to, the number average molecular weight (Mn). The only situation in which the weight average molecular weight and the number average molecular weight are equal is when a polymer consists only of chains with equal molecular weight. However, this never happens in a synthetic polymer, since it is difficult to control the polymerization process up to a molecular level with accuracy to a hundred percent.

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Updated: Jun 24, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

Predicción del peso de la fórmula mediante espectroscopia de RMN ordenada por difusión de referencia interna (DOSY).

Deyu Li1, Gerald Kagan, Russell Hopson

  • 1Department of Chemistry, Brown University, Providence, Rhode Island 02912, USA.

Journal of the American Chemical Society
|March 28, 2009
PubMed
Resumen
Este resumen es generado por máquina.

Este estudio introduce un método DOSY correlacionado de referencia interna para determinar el peso de fórmula (PV) de moléculas desconocidas. Esta técnica práctica caracteriza con precisión las especies en diversos disolventes y concentraciones.

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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Área de la Ciencia:

  • Química Analítica La Química Analítica es la
  • La Química Física es la química física.
  • Química orgánica es la química orgánica.

Sus antecedentes:

  • El peso de la fórmula (FW) es crucial para caracterizar los intermediarios reactivos y los complejos organometálicos.
  • La determinación precisa de las ayudas FW en la comprensión de la composición, la agregación y los estados de solvación.
  • Los métodos existentes pueden tener limitaciones en diversas condiciones de disolvente y concentración.

Objetivo del estudio:

  • Desarrollar y validar un método DOSY correlacionado de referencia interna para el cálculo de FW.
  • Para evaluar la precisión y aplicabilidad del método en diferentes disolventes y concentraciones.
  • Proporcionar directrices para la implementación exitosa de esta nueva técnica de caracterización.

Principales métodos:

  • Espectroscopia Ordenada por Difusión Utilizada (DOSY) con un estándar de referencia interno.
  • Empleado DOSY correlacionado para calcular el peso de fórmula (FW) de especies desconocidas.
  • Investigó la influencia del disolvente, la concentración y la viscosidad de la solución en la precisión.

Principales resultados:

  • Se obtuvieron excelentes correlaciones tanto para moléculas pequeñas (DIPA) como para complejos organometálicos (agregado 1).
  • Demostró que las tasas de difusión relativa se correlacionan inversamente con la viscosidad de la solución, alineándose con la ecuación de Stokes-Einstein.
  • La precisión de la predicción encontrada (r ^ 2, diferencia en %) está vinculada a los cambios de densidad, mejorando con la disminución de la densidad.

Conclusiones:

  • El método DOSY correlacionado de referencia interna proporciona un enfoque práctico y preciso para la determinación de FW.
  • El método es versátil, aplicable a diversas moléculas y complejos en diferentes condiciones de solución.
  • Esta técnica ofrece una herramienta valiosa para caracterizar especies químicas desconocidas.