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

A technology of triethylene glycol dinitrate and hydrogen nuclear magnetic resonance spectroscopy, which is applied in the directions of using nuclear magnetic resonance for analysis, material analysis by resonance, and measuring devices, etc., can solve the limitation of high cost, simple and rapid testing requirements for quantitative analysis. , the method is cumbersome and other problems, to achieve the effect of simple and rapid testing, high sensitivity, and low 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 content of mixed nitrate of triethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum
  • Method for measuring moisture content of mixed nitrate of triethylene glycol dinitrate and nitroglycerin through nuclear magnetic resonance hydrogen spectrum
  • Method for measuring moisture content of mixed nitrate of triethylene 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] TEGDN / NG mixed nitrate 1 Construction of H NMR spectrum

[0031] 1.1 Instruments and samples

[0032] BrukerAscend 800 superconducting nuclear magnetic resonance spectrometer (German BRUKER company); MettlerToledoXP6 type one hundred thousandth balance (Switzerland METTLER company); deuterated dimethyl sulfoxide (deuterated 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); TEGDN / NG mixed nitrate (Xi’an Institute of Modern Chemistry, batch number 170903)

[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 0.6ml of deuterated dimethyl sulfoxide, mix well and seal it with a parafilm, and use the prepared NMR sample directly for 1 H NMR test. After the test is over, remove the NMR sample...

Embodiment 2

[0051] Determination of water content in different batches of TEGDN / NG mixed nitrate by 1H NMR

[0052] Accurately weigh 5.3mg of internal standard benzene into a 5mm NMR tube, then add 0.6ml 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 15 mg of mixed nitrates and mix thoroughly, seal with a sealing film, and then carry out the sample under the same test conditions 1 H NMR test. According to the same method, three batches of different batches of TEGDN / 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.

[0053] Table 3 Determination of moisture content of di...

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Abstract

The invention discloses a method for measuring the moisture content of mixed nitrate of triethylene glycol dinitrate (TEGDN) 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 sample solution, 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 standardsample, 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 triethylene glycol dinitrate (TEGDN) 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 triethylene glycol dinitrate (TEGDN) and nitroglycerin (NG) 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. It is not only a good plasticizer for nitrocellulose, but also the main energy component in the propellant composition. It plays an important role in making semi-rigid nitrocellulose into extrudable materials and reducing the glass transition temperature. Indispensable important component. Especially triethylene glycol dinitrate (TEGDN) and nitroglycerin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/084
Inventor 刘可宁艳利王民昌陈智群常海张皋徐敏苏鹏飞胡银
Owner XIAN MODERN CHEM RES INST
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