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

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

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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

1.3K
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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Updated: Jan 13, 2026

Quantitative 31P NMR Analysis of Lignins and Tannins
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高信頼性チオール基分析のための定量31P NMR分光法の進歩

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
まとめ

TMDP試薬を用いた新しい31P NMR法は、ポリマーおよび材料中のチオールを正確に定量する。この技術は、複雑または劣化したチオールサンプルに対しても、従来の測定法よりも優れた選択性を提供する。

キーワード:
31P NMRチオール定量TMDP試薬ポリマー材料科学分析化学

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科学分野:

  • 高分子化学
  • 材料科学
  • 分析化学

背景:

  • 正確なチオール定量は、ポリマーおよび材料合成におけるチオール-X-リゲーションにとって重要である。
  • Ellmanアッセイなどの従来の測定法は、疎水性または多官能チオールには限界がある。

研究 の 目的:

  • 広く適用可能で正確なチオール定量法を開発すること。
  • チオール分析のための31P NMR分光法の拡張。

主な方法:

  • ホスファイト化試薬として2-クロロ-4,4,5,5-テトラメチル-1,3,2-ジオキサホスホラン（TMDP）を使用した。
  • チオール定量のために31P NMR分光法を適用した。
  • Ellmanアッセイおよび1H NMR分光法と比較してこの方法を検証した。

主要な成果:

  • TMDPベースの31P NMR法は、チオール定量において高い特異性と安定した読み取り値を提供する。
  • この方法は、8000 g・mol-1までのポリマー多官能チオールを含む幅広い基質に適用可能である。
  • 従来の測定法と比較して、特に工業グレードのチオールにおいて、優れた選択性と分解能を示した。

結論:

  • TMDPを可能にした31P NMRは、多様な化学的文脈におけるチオール定量のための信頼できるツールである。
  • この方法は、ヒドロキシ基およびカルボキシ基官能基に関する同時情報を提供する。
  • 材料科学および高分子化学におけるチオール分析の新しい標準を確立する。