Method for measuring moisture content of mixed nitrate of diethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum

A technology of diethylene glycol dinitrate and hydrogen nuclear magnetic resonance spectroscopy, which is applied in the directions of analysis by nuclear magnetic resonance, material analysis by resonance, and measurement devices, can solve the limitation of high cost, simple and rapid test requirements for quantitative analysis. , the method is cumbersome and other problems, to solve the sensitive and easy to explode, the test is simple and rapid, and the amount of use is small.

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 content of mixed nitrate of diethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum
  • Method for measuring moisture content of mixed nitrate of diethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum
  • Method for measuring moisture content of mixed nitrate of diethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum

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Experimental program
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Effect test

Embodiment 1

[0030] DEGDN / NG mixed nitrate 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); Benzene purity standard substance (Tianjin Metrology Supervision and Testing Science Research Institute, batch number 0401); DEGDN / NG mixed nitrate (Xi'an Institute of Modern Chemistry, batch number 180405)

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

[0034] Accurately weigh 5-15mg of the internal standard benzene standard substance into a 5mm NMR tube, then add 0.5ml deuterated dimethyl sulfoxide, mix well and seal with a parafilm, and use the prepared NMR sample directly for 1 H NMR test. After the test is over, remove the NMR sample tube that has c...

Embodiment 2

[0050] Determination of water content in different batches of DEGDN / NG mixed nitrate by 1H NMR

[0051] Accurately weigh 6.5mg of internal standard benzene into 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, test parameters and conditions are: observation frequency 800.3MHz, measurement temperature 300K, 90° pulse, spectrum width 3μs, sampling data points 65536, scan times 128 times, delay time 30s. Then remove the NMR sample tube after the test, add 17mg of mixed nitrates and mix thoroughly, seal with a parafilm, and then test the sample under the same test conditions 1 H NMR test. According to the same method, three batches of different batches of DEGDN / NG mixed nitrate samples were tested, the NMR spectra were recorded, and the moisture content was calculated. The results are shown in Table 3 below.

[0052] Table 3 Determination of moisture content of different...

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Abstract

The invention discloses a method for measuring the moisture content of mixed nitrate of diethylene glycol dinitrate (DEGDN) and nitroglycerin (NG) through a nuclear magnetic resonance hydrogen spectrum. Quantitative detection of trace moisture is achieved based on a nuclear magnetic hydrogen spectrum internal standard method. The specific steps comprise: (1) configuring an internal standard samplesolution, and detecting the nuclear magnetic resonance hydrogen spectrum; (2) adding a mixed nitrate sample to be measured, and detecting the nuclear magnetic resonance hydrogen spectrum; and (3) performing affiliation on each characteristic peak in the nuclear magnetic resonance hydrogen spectrum, determining the characteristic peak of water and the characteristic peak of the internal standard sample, respectively performing integration, and substituting into a corresponding formula to calculate the corresponding moisture content. The method has the advantages of simple and convenient operation, small sample amount, good repeatability and the like, can be used for performing quantitative detection on the moisture content contained in the mixed nitrate of diethylene glycol dinitrate (DEGDN) and nitroglycerin (NG) quickly, and can used for directionally solving the key problems of relevant quality control in the application of explosives and powders.

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 mixed nitrates of diethylene glycol dinitrate (DEGDN) and nitroglycerin (NG) by hydrogen nuclear magnetic resonance spectroscopy, which belongs to the analysis and detection of propellant and explosive products field. 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) and nitroglycerin (NG) in the form of mixed nitrates, as the main energy components in the propellant composition, become extrudable materials for semi-rigid nitrocellulose and reduce The glass transition temperature plays an important role. Due to its low price, good low-temperature mechanical properties, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/084
Inventor 刘可徐敏张皋常海陈智群宁艳利王民昌苏鹏飞康莹朱一举
Owner XIAN MODERN CHEM RES INST
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