A kind of method for measuring diethylene glycol dinitrate moisture content by proton nuclear magnetic resonance spectrum

A technique of diethylene glycol dinitrate and proton nuclear magnetic resonance spectroscopy, which is applied in the fields of nuclear magnetic resonance analysis, material analysis through resonance, and measuring devices, can solve the problem of high cost of quantitative analysis work, cumbersome methods, simple and rapid Limitation of test requirements and other issues, to achieve the effect of solving sensitive and explosive, less dosage, simple and rapid testing

Active Publication Date: 2021-07-27
XIAN MODERN CHEM RES INST
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

As a relative measurement method, near-infrared spectroscopy has high test sensitivity, but its calibration requires one-to-one corresponding standard substances, and corresponding working curves are drawn. The corresponding quantitative analysis is also costly and cumbersome. For simple and rapid testing Requirements are also limited

Method used

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  • A kind of method for measuring diethylene glycol dinitrate moisture content by proton nuclear magnetic resonance spectrum
  • A kind of method for measuring diethylene glycol dinitrate moisture content by proton nuclear magnetic resonance spectrum
  • A kind of method for measuring diethylene glycol dinitrate moisture content by proton nuclear magnetic resonance spectrum

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Experimental program
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Embodiment 1

[0030] Diethylene glycol dinitrate 1 Construction of H NMR spectrum

[0031] 1.1 Instruments and samples

[0032] Bruker Ascend 800 superconducting nuclear magnetic resonance spectrometer (Germany BRUKER company); Mettler ToledoXP6 type 1 / 100,000 balance (Switzerland METTLER company); deuterated dimethyl sulfoxide (deuterium degree > 99.8%, American CIL company) ; 5mm standard NMR sample tube (NORELL, USA); high-purity hexamethyldisiloxane (Anaiji Chemical, purity 99%); diethylene glycol dinitrate (Xi'an Institute of Modern Chemistry).

[0033] 1.2 Preparation and determination of samples to be tested

[0034] Accurately weigh 5-15 mg of the internal standard hexamethyldisiloxane into a 5mm NMR tube, then add 0.5ml of deuterated dimethyl sulfoxide, mix well and seal with a parafilm, and use the prepared NMR samples directly for 1 H NMR test. After the test is over, remove the NMR sample tube that has completed the test, add 10-30 mg of diethylene glycol dinitrate and mix w...

Embodiment 2

[0050] Determination of Moisture Content in Different Batches of Diethylene Glycol Dinitrate by 1H NMR Spectroscopy

[0051] Accurately weigh 5.3 mg of the internal standard hexamethyldisiloxane in a 5mm NMR tube, then add 0.6ml of deuterated dimethyl sulfoxide, mix well and seal with a parafilm, and use the prepared NMR sample directly for 1 H NMR test, the test parameters and conditions are: observation frequency 800.3MHz, measurement temperature 300K, 90° pulse, spectral width 3μs, sampling data points 65536, number of scans 64 times, delay time 40s. Then remove the NMR sample tube after the test, add 12 mg of diethylene glycol dinitrate and mix well, add a sealing film to seal, and then test the sample under the same test conditions 1 H NMR test. According to the same method, three batches of diethylene glycol dinitrate samples with different batch numbers were detected, the nuclear magnetic resonance spectra were recorded, and the moisture content was calculated. The res...

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Abstract

The invention discloses a method for measuring the water content of diethylene glycol dinitrate (DEGDN) by hydrogen nuclear magnetic resonance spectroscopy. The quantitative detection of trace moisture is realized based on the hydrogen nuclear magnetic resonance internal standard method, and the specific steps include: (1) internal standard (2) adding and proton nuclear magnetic resonance spectrum detection of diethylene glycol dinitrate sample to be measured; (3) assigning each characteristic peak in the proton nuclear magnetic resonance spectrum, Determine the characteristic peaks of water and the characteristic peaks of the internal standard, and integrate them separately, and substitute into the relevant formula to calculate the corresponding water content. The method has the advantages of simple operation, less sample amount, and good repeatability. It can quickly and quantitatively detect the moisture content of diethylene glycol dinitrate, and can solve key problems related to quality control in the application of propellants and explosives.

Description

technical field [0001] The invention belongs to the field of measurement and detection of energetic materials, in particular to a method for measuring the water content of diethylene glycol dinitrate (DEGDN) by hydrogen nuclear magnetic resonance spectroscopy, and belongs to the field of analysis and detection of propellant and explosive products. Background technique [0002] As an excellent plasticizer, nitrate esters are widely used in the fields of double-base propellants and composite propellants due to their better oxygen balance and good combustion and explosive properties. In particular, diethylene glycol dinitrate (DEGDN), as the main energy component in the propellant composition, plays an important role in making semi-rigid nitrocellulose an extrudable material and reducing the glass transition temperature. Good mechanical properties and low burning rate of basic components have been widely used as energetic plasticizers in a new generation of high-energy propella...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/084
Inventor 刘可王民昌宁艳利康莹张丽涵徐敏胡银常海张皋陈智群
Owner XIAN MODERN CHEM RES INST
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