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Method for measuring moisture contents of diethylene glycol dinitrate by H nuclear magnetic resonance

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

Active Publication Date: 2018-12-18
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • 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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  • Method for measuring moisture contents of diethylene glycol dinitrate by H nuclear magnetic resonance
  • Method for measuring moisture contents of diethylene glycol dinitrate by H nuclear magnetic resonance
  • Method for measuring moisture contents of diethylene glycol dinitrate by H nuclear magnetic resonance

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Experimental program
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Effect test

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 moisture contents of diethylene glycol dinitrate (DEGDN) by H nuclear magnetic resonance, and realizes the quantitative detection of trace moisture on the basis of an H nuclear magnetic resonance internal standard method. The method comprises the following specific steps that: (1) configuring internal standard substance specimen solution, and detecting the H nuclear magnetic resonance; (2) adding a DEGDN sample to be measured, and detecting the H nuclear magnetic resonance; and (3) carrying out affiliation on each characteristic peak in the Hnuclear magnetic resonance, determining the characteristic peak and the internal standard substance characteristic peak of water, independently carrying out integration, and substituting a relevant formula to calculate corresponding moisture contents. The method has the advantages of being simple in operation, small in sample amount, good in repeatability and the like, the moisture content in theDEGDN can be quickly quantitatively detected, and a key problem of relative quality control in the application of explosives and powders can be solved in a targeted way.

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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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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