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Nuclear magnetic resonance method for measuring all hydrogen-hydrogen coupling constants in molecule

A technology of nuclear magnetic resonance and coupling constant, which is applied in the direction of using nuclear magnetic resonance for analysis, measurement device, material analysis by resonance, etc., to achieve the effect of promoting application

Inactive Publication Date: 2017-07-07
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method can only measure the coupling constants in the coupled network of one selected core at a time

Method used

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  • Nuclear magnetic resonance method for measuring all hydrogen-hydrogen coupling constants in molecule
  • Nuclear magnetic resonance method for measuring all hydrogen-hydrogen coupling constants in molecule
  • Nuclear magnetic resonance method for measuring all hydrogen-hydrogen coupling constants in molecule

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Embodiment Construction

[0030] Below in conjunction with accompanying drawing and embodiment, the present invention will be further described:

[0031] This embodiment uses the Varian 500MHz nuclear magnetic resonance spectrometer equipped with Z direction gradient field, and the sample is a solution of 1mol / L bromobutane dissolved in deuterated chloroform, using such as figure 1 The pulse sequence shown.

[0032] Step 1: Collect one-dimensional hydrogen NMR spectrum of a sample, such as figure 2 shown;

[0033] Step 2: Measure the 90-degree hard pulse width of the sample, which is 13.8 μs;

[0034] Step 3: Determine the frequency range of the one-dimensional hydrogen spectrum of the sample, the frequency range of the one-dimensional hydrogen spectrum in this embodiment is 0.3ppm-4.2ppm;

[0035] Step 4: The center frequency of the frequency range of the one-dimensional hydrogen spectrum of the sample is used as the excitation center of the soft pulse. The soft pulse width is determined accordin...

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Abstract

The invention provides a nuclear magnetic resonance method for measuring all hydrogen-hydrogen coupling constants in a molecule. The nuclear magnetic resonance method comprises the following steps: firstly applying one 90-degree hard pulse to rotate a magnetization vector to an XY plane from a Z direction, setting a sampling point at one fixed moment delta after the 90-degree hard pulse; enabling a selective 180-degree soft pulse applied at the same time with Z direction magnetic field gradient to move between the 90-degree hard pulse and the sampling point along with variation of indirect dimension evolution time t1; under the action of the magnetic field gradient, overturning different nucleuses at different spatial positions by the selective 180-degree soft pulse; acquiring chemical displacement information and spatial position information at the same time by adopting an EPSI sampling module, so that couplings of other nucleuses and the nucleus overturned by the 180-degree soft pulse at the same layer can be obtained at different layers, the couplings can show up split peaks at an indirect dimension, and corresponding J coupling constants can be measured from the split peaks.

Description

technical field [0001] The invention relates to a nuclear magnetic resonance method, in particular to a method for accurately measuring the nuclear magnetic resonance multidimensional spectrum of hydrogen-hydrogen J coupling constants of all coupling networks in molecules. Background technique [0002] The interaction between spin nuclei and spin nuclei is an important information in NMR spectra, which plays an important role in molecular structure analysis. Among them, the triple bond J coupling between hydrogen and hydrogen is widely used in the study of molecular conformation because its coupling constant is related to the dihedral angle formed by the triple bond. However, the coupling constants between hydrogen and hydrogen are often submerged in one-dimensional NMR spectra due to narrow chemical shift distributions, complex split peak modes, and large spectral peak linewidths. A recently proposed SECT NMR two-dimensional spectrum method (L.Lin, Z.Wei, Y.Lin and Z.Chen,...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/087
Inventor 林雁勤曾庆陈金永林良杰陈忠
Owner XIAMEN UNIV
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