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A method for sample preparation and loading before solid-state NMR characterization of gas hydrate

A technology for gas hydrates and solids, which is applied in the direction of nuclear magnetic resonance analysis, measuring devices, instruments, etc., can solve the problems of unable to complete the nuclear magnetic test, cover damage, etc., and achieve efficient and fast sample preparation, strong and not easy to break, strengthened Efficiency effect

Active Publication Date: 2021-04-02
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for sample preparation and loading before solid-state NMR characterization of gas hydrate. The sample preparation is efficient and fast, which is helpful to quickly and efficiently complete the solid-state NMR test of gas hydrate, and accurately obtain the gas hydrate. Structural information, information on the structure and composition changes of gas hydrates in the process of formation and decomposition, exploring the mechanism of gas hydrate formation and decomposition, and solving the problem of frosting in the sample preparation process in liquid nitrogen, which caused damage to the cover of the sealed rotor and could not be completed NMR Test Questions

Method used

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  • A method for sample preparation and loading before solid-state NMR characterization of gas hydrate
  • A method for sample preparation and loading before solid-state NMR characterization of gas hydrate
  • A method for sample preparation and loading before solid-state NMR characterization of gas hydrate

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Embodiment 1

[0031] The performance parameters of the solid-state NMR ultra-low temperature special cover for solid-state NMR characterization of the gas hydrate structure in this embodiment are: working temperature: -196°C to room temperature, and rotation speed: 0-5KHz. as methane gas hydrate 13 Take the CNMR test as an example.

[0032] A method for sample preparation and sample loading before solid-state NMR characterization of gas hydrates, the method comprising the following steps,

[0033] 1) Take a 5L insulated box with a cover, add 2.5L of liquid nitrogen, put the rotor, special cover for solid nuclear magnetic ultra-low temperature, sampling spoon, mortar, sample loading tool, and cover loading tool into liquid nitrogen for precooling;

[0034] 2) Add 20mL of liquid nitrogen to the pre-cooled mortar in step 1), put the methane gas hydrate generated in the reaction device into the mortar, grind finely, and then add 20mL of liquid nitrogen to ensure that the methane Gas hydrates ...

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Abstract

The invention discloses a method for preparing and loading a sample before solid nuclear magnetism of gas hydrate. According to the method, the sample in efficiently and rapidly prepared, so that thesample is protected to the maximum extent; a lid is firm and unlikely to be damaged, the solid nuclear magnetism test of the gas hydrate can be rapidly and efficiently finished, the accurate structural information of the gas hydrate and the structural and constitutional change information of the gas hydrate in the generation and decomposition processes can be acquired, and the generation and decomposition mechanisms of the gas hydrate can be explored, so that the problems that the lid of a sealing rotor is damaged due to the frosting in the sample preparation process of liquid nitrogen, and the nuclear magnetism test cannot be finished are solved.

Description

Technical field: [0001] The invention relates to the technical field of solid nuclear magnetic characterization, in particular to a method for sample preparation and loading before solid nuclear magnetic characterization of gas hydrates. Background technique: [0002] Natural gas hydrate is an ice-like crystal formed by gas and water and stable at low temperature and high pressure. The microscopic characterization of gas hydrates provides important reference data for the study of gas hydrate formation and decomposition mechanisms for gas hydrate accumulation mechanisms, gas production, storage and transportation. [0003] Solid-state NMR spectroscopy provides valuable information such as structure type, guest molecular composition, and cage occupancy for the study of gas hydrates. When the gas hydrate is taken out and characterized under normal pressure, it is easy to decompose. Therefore, sample loading should be carried out in liquid nitrogen protection to avoid sample d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/087
Inventor 付娟苏秋成
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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