Method and device for measuring spin lattice relaxation time

A technology of relaxation time and spin lattice, which is applied in the analysis of nuclear magnetic resonance, etc., can solve the problems of unsuitable molecules, reduced polarization transfer efficiency, and inability to achieve measurement, etc., and achieves a high universal effect

Active Publication Date: 2019-06-25
SUZHOU UNIV
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Problems solved by technology

When the heteronuclear dipole coupling is strong, the cross-polarization process can achieve 1 H to 13 The polarization transfer of C, but when the dipole coupling effect is weak, the polarization transfer efficiency will decrease. This is the principle of the system with relatively strong mobility, so the Torchia experiment is not suitable for the system with strong molecular mobility, that is, heteronuclear For systems with weak dipole coupling 13 Determination of the spin-lattice relaxation time of C
[0004] For multiphase systems with large differences in molecular local mobility (that is, systems with both rigid and flexible phases) or containing 1 H / not included 1 For the blended sample of H, neither the IR nor the Torchia method can achieve the determination of all components in the sample system. 13 CT 1 Measurement

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  • Method and device for measuring spin lattice relaxation time
  • Method and device for measuring spin lattice relaxation time
  • Method and device for measuring spin lattice relaxation time

Examples

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example 1

[0087] Example 1: In an alanine / adamantane blend 13 CT 1 Determination of value

[0088] The reason for choosing the alanine / adamantane blend as the sample system is that alanine is a 1 Rigid molecules with H atoms are more suitable to be determined by Torchia experiment 13 CT 1 value; and according to the structural characteristics of adamantane molecules, its molecules have high mobility, so its 13 C- 1 The dipole coupling effect of H is relatively weak, so it is more suitable to use IR (inversion-recovery method) to test its 13 CT 1 value. Therefore, alanine / adamantane was selected as a system with large differences in molecular local mobility to evaluate the accuracy of DP-Torchia.

[0089] The specific experimental operation is: put the alanine / adamantane blend solid powder into the solid NMR sample tube and place it in the probe, retrieve the DP-Torchia pulse sequence file, set the appropriate experimental parameters, and collect the DP-Torchia spectrum . After...

example 2

[0094] Example 2: In polyvinyl alcohol / polytetrafluoroethylene blends 13 CT 1 Determination of value

[0095] The reason for choosing polyvinyl alcohol / polytetrafluoroethylene blend as the sample system is that polyvinyl alcohol is 13 C- 1 H system, there is heteronuclear dipole coupling effect, it is more suitable to use Torchia experiment to determine its 13 CT 1 Value; PTFE system does not contain 1 H, so there is no 13 C- 1 H dipole coupling effect, in the traditional method, IR experiments are generally used to determine the groups 13 CT 1 value. However, this method can simultaneously determine the 1 H / not included 1 Each group of the blend system of H 13 CT 1 value, so polyvinyl alcohol / polytetrafluoroethylene was selected as the 1 H / not included 1 H blend system to evaluate the performance of DP-Torchia.

[0096] The specific experimental operation is: put the solid powder of polyvinyl alcohol / polytetrafluoroethylene blend into the solid NMR sample tube...

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Abstract

The invention discloses a method and a device for determining the spin lattice relaxation time. The method comprises the steps that a sample to be tested is determined based on a preset pulse sequenceto acquire the original data of a pseudo two-dimensional spectrum; phase and baseline correction is carried out on the pseudo two-dimensional spectrum after Fourier transform to acquire a corrected two-dimensional spectrum; in the corrected pseudo two-dimensional spectrum, the 13C peak of each group in a sample to be tested are integrated to acquire the integrated area of the peaks correspondingto different delay times; and the data, which change with the delay time, of the integrated area of the peaks corresponding to different delay times are fitted to acquire the spin lattice relaxation time of the sample to be tested. A predetermined pulse sequence includes the determination of the part with high molecule local mobility or the part without 1H in the sample to be tested, and the determination of the hydrogenous rigid part with weak molecule local mobility in the sample to be tested. The spin lattice relaxation time of 13C for each group in a blend system is determined based on onemeasurement.

Description

technical field [0001] The invention relates to the technical field of solid-state nuclear magnetic resonance, in particular to a spin-lattice relaxation time measurement method and device. Background technique [0002] The measurement of spin-lattice relaxation time constitutes an important aspect of NMR (Nuclear Magnetic Resonance, nuclear magnetic resonance) experiment. This is because the spin-lattice relaxation time characterizes important information about molecular motion to a certain extent, and this information is difficult for chemists to obtain by other means. [0003] For the measurement of a group in a sample system 13 The traditional measurement methods for the spin-lattice relaxation time of C mainly include inversion-recovery experiments (IR, inverse-recovery) and Torchia experiments. Regarding the pulse sequence for IR experiments such as figure 1 As shown in (a), it is mainly suitable for samples with strong molecular mobility or without 1 of each group...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 舒婕王宁朱惠芳徐凌云严丽娟
Owner SUZHOU UNIV
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