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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

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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...
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NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

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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...
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Other Nuclides: 31P, 19F, 15N NMR01:16

Other Nuclides: 31P, 19F, 15N NMR

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Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a...
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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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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...
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NMR Spectroscopy Of Amines01:19

NMR Spectroscopy Of Amines

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In proton NMR spectroscopy, primary amines and secondary amines showcase their N–H protons as a broad signal in the chemical shift range between δ 0.5 and 5 ppm. The exact position in this range depends on several factors, including sample concentration, hydrogen bonding, and the type of solvent used. Since amine protons undergo fast proton exchange in solution, the protons are labile and therefore do not participate in any splitting with adjacent protons. Thus, the observed peak is...
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¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

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A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
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Video Experimental Relacionado

Updated: Jan 13, 2026

Quantitative 31P NMR Analysis of Lignins and Tannins
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Avance de la espectroscopia de RMN cuantitativa de 31P para el análisis fiable del grupo tiol

Keven Walter1, Dominik P Hoch1, Enrico C Heyl1

  • 1Humboldt-Universität zu Berlin, Department of Chemistry, Laboratory for Organic Synthesis of Functional Systems, Brook-Taylor-Str. 2, 12489 Berlin, Germany.

ACS macro letters
|January 7, 2026
PubMed
Resumen

Un nuevo método de RMN de 31P que utiliza el reactivo TMDP cuantifica con precisión los tioles en polímeros y materiales. Esta técnica ofrece una selectividad superior a los ensayos tradicionales, incluso para muestras de tiol complejas o degradadas.

Palabras clave:
cuantificación de tiolesRMN de 31PTMDPsíntesis de polímerosciencia de materialesespectroscopia de RMNanálisis de tiolesensayos convencionalestioles multifuncionalestioles hidrofóbicos

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Área de la Ciencia:

  • Química de polímeros
  • Ciencia de materiales
  • Química analítica

Sus antecedentes:

  • La cuantificación precisa de tioles es crucial para la tiol-X-ligación en la síntesis de polímeros y materiales.
  • Los métodos convencionales como la prueba de Ellman tienen limitaciones con tioles hidrofóbicos o multifuncionales.

Objetivo del estudio:

  • Desarrollar un método preciso y de aplicación generalizada para la cuantificación de tioles.
  • Extender la espectroscopia de RMN de 31P para el análisis de tioles.

Principales métodos:

  • Se utilizó 2-cloro-4,4,5,5-tetrametil-1,3,2-dioxafosfolano (TMDP) como reactivo de fosfitilación.
  • Se aplicó espectroscopia de RMN de 31P para la cuantificación de tioles.
  • Se validó el método frente al ensayo de Ellman y la espectroscopia de RMN de 1H.

Principales resultados:

  • El método de RMN de 31P basado en TMDP proporciona alta especificidad y lectura estable para la cuantificación de tioles.
  • El método es aplicable a una amplia gama de sustratos, incluidos multitoles poliméricos de hasta 8000 g·mol-1.
  • Demostró una selectividad y resolución superiores en comparación con los ensayos convencionales, especialmente para tioles de grado técnico.

Conclusiones:

  • La RMN de 31P habilitada por TMDP es una herramienta fiable para la cuantificación de tioles en diversos contextos químicos.
  • Este método ofrece información simultánea sobre la funcionalidad hidroxilo y carboxilo.
  • Establece un nuevo estándar para el análisis de tioles en la ciencia de materiales y la química de polímeros.