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

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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.
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Chemical Shift: Internal References and Solvent Effects01:17

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NMR Spectroscopy Of Amines01:19

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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

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Updated: Jan 13, 2026

Quantitative 31P NMR Analysis of Lignins and Tannins
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Advancing Quantitative 31P NMR Spectroscopy for Reliable Thiol Group Analysis.

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
Summary
This summary is machine-generated.

A new 31P NMR method using TMDP reagent accurately quantifies thiols in polymers and materials. This technique offers superior selectivity over traditional assays, even for complex or degraded thiol samples.

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Area of Science:

  • Polymer Chemistry
  • Materials Science
  • Analytical Chemistry

Background:

  • Accurate thiol quantification is crucial for thiol-X-ligation in polymer and materials synthesis.
  • Conventional methods like Ellman's test have limitations with hydrophobic or multifunctional thiols.

Purpose of the Study:

  • To develop a broadly applicable and accurate method for thiol quantification.
  • To extend 31P NMR spectroscopy for thiol analysis.

Main Methods:

  • Utilized 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane (TMDP) as a phosphitylation reagent.
  • Applied 31P NMR spectroscopy for thiol quantification.
  • Validated the method against Ellman's assay and 1H NMR spectroscopy.

Main Results:

  • The TMDP-based 31P NMR method provides high specificity and stable readout for thiol quantification.
  • The method is applicable to a wide range of substrates, including polymeric multi thiols up to 8000 g·mol-1.
  • Demonstrated superior selectivity and resolution compared to conventional assays, especially for technical-grade thiols.

Conclusions:

  • The TMDP-enabled 31P NMR is a reliable tool for thiol quantification in diverse chemical contexts.
  • This method offers simultaneous insights into hydroxy and carboxyl functionality.
  • Establishes a new standard for thiol analysis in materials science and polymer chemistry.