A kind of method for measuring 1,2-propanediol dinitrate moisture content by proton nuclear magnetic resonance

A technology of propylene glycol dinitrate and hydrogen 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 high cost of quantitative analysis, the limitation of simple and rapid testing requirements, and the cumbersome methods and other problems, to achieve the effect of simple and rapid testing, high sensitivity, and less dosage

Active Publication Date: 2021-07-23
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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  • A kind of method for measuring 1,2-propanediol dinitrate moisture content by proton nuclear magnetic resonance
  • A kind of method for measuring 1,2-propanediol dinitrate moisture content by proton nuclear magnetic resonance
  • A kind of method for measuring 1,2-propanediol dinitrate moisture content by proton nuclear magnetic resonance

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Experimental program
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Embodiment 1

[0030] 1,2-Propanediol 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%); 1,2-propanediol dinitrate (Xi'an Institute of Modern Chemistry).

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

[0034] Accurately weigh 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 been tested, add 30mg of 1,2-propanediol dinitrate and mix well, add a sealing ...

Embodiment 2

[0050] Determination of Moisture Content in Different Batches of 1,2-Propanediol Dinitrate by 1H NMR

[0051] Accurately weigh 5.9 mg of the internal standard hexamethyldisiloxane 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, 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 tested NMR sample tube, add 13mg of 1,2-propanediol dinitrate and mix thoroughly, seal with a sealing film, and then test the sample under the same test conditions 1 H NMR test. According to the same method, three batches of 1,2-propanediol dinitrate samples with different batch numbers were detected, the nuclear magnetic resonance spectra were recorded, and the moisture content was calculated. The results are shown in Tabl...

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Abstract

The invention discloses a method for measuring the water content of 1,2-propylene glycol dinitrate (PGDN) by hydrogen nuclear magnetic resonance spectroscopy. The quantitative detection of trace moisture is realized based on the hydrogen nuclear magnetic resonance internal standard method. The specific steps include: (1) Configuration and proton nuclear magnetic resonance spectrum detection of standard substance sample solution; (2) adding and proton nuclear magnetic resonance spectrum detection of 1,2 propanediol dinitrate sample to be measured; (3) carrying out each characteristic peak in proton nuclear magnetic resonance spectrum Attribution, determine the characteristic peaks of water and the characteristic peaks of the internal standard, and integrate them respectively, and substitute into the relevant formula to calculate the corresponding water content. The method has the advantages of simple operation, small sample volume, and good repeatability. It can quickly and quantitatively detect the moisture content of 1,2-propanediol dinitrate, and can solve key problems related to quality control in the application of 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 moisture content of 1,2-propanediol dinitrate (PGDN) 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 ester is widely used in the fields of composite propellants and double-base propellants because of its good oxygen balance and good combustion and explosive properties. In particular, 1,2-propanediol dinitrate (PGDN), as the main energy and plasticizing component in the propellant composition, plays an important role in making semi-rigid nitrocellulose an extrudable material and reducing the glass transition temperature. It is widely used as an energetic plasticizer in a new generation of high-energy propellants due to its low price, low burning rate of basic compon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/084
Inventor 刘可王民昌徐敏张丽涵陈智群宁艳利赵嘉静常海张皋
Owner XIAN MODERN CHEM RES INST
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