A kind of method for the determination of nitroglycerin moisture content by hydrogen nuclear magnetic resonance spectroscopy

A technique of proton nuclear magnetic resonance spectroscopy and nitroglycerin, which is applied to analysis by nuclear magnetic resonance, material analysis by resonance, measurement device, etc. , to achieve the effect of less dosage, solving sensitive and easy explosion, and easy and rapid testing

Active Publication Date: 2021-07-23
XIAN MODERN CHEM RES INST
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  • 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 the determination of nitroglycerin moisture content by hydrogen nuclear magnetic resonance spectroscopy
  • A kind of method for the determination of nitroglycerin moisture content by hydrogen nuclear magnetic resonance spectroscopy
  • A kind of method for the determination of nitroglycerin moisture content by hydrogen nuclear magnetic resonance spectroscopy

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Experimental program
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Effect test

Embodiment 1

[0029] Nitroglycerin 1 Construction of H NMR spectrum

[0030] 1.1 Instruments and samples

[0031] 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); Nitroglycerin (Xi'an Institute of Modern Chemistry)

[0032] 1.2 Preparation and determination of samples to be tested

[0033] Accurately weigh 10 mg of the internal standard benzene standard substance 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. After the test is over, remove the NMR sample tube that has been tested, add 20 mg of nitroglyceri...

Embodiment 2

[0048] Determination of Moisture Content in Different Batches of Nitroglycerin by H NMR Spectroscopy

[0049] Accurately weigh 5.0mg of internal standard benzene 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, 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 12.0 mg of nitroglycerin 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 different batches of nitroglycerin samples were tested, the nuclear magnetic resonance spectra were recorded, and the moisture content was calculated. The results are shown in Table 3 below.

[0050] Table 3 Determination of moisture c...

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Abstract

The invention discloses a method for measuring the water content of nitroglycerin by hydrogen nuclear magnetic resonance spectroscopy. The quantitative detection of trace moisture is realized based on the hydrogen nuclear magnetic resonance spectroscopy internal standard method. The specific steps include: (1) hydrogen nuclear magnetic resonance spectroscopy detection and internal standard test (2) adding of the nitroglycerin sample to be tested and proton nuclear magnetic resonance spectrum detection; (3) assigning each characteristic peak in the proton nuclear magnetic resonance spectrum, determining the characteristic peak of water and the characteristic peak of the internal standard substance, and Integrate separately and substitute into relevant formulas to calculate the corresponding moisture content. The method has the advantages of good safety, simple operation, good repeatability, etc., and can quickly and quantitatively detect the moisture content in nitroglycerin, and specifically solve the key problems related to quality control in the application of propellant 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 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] Since its inception, nitroglycerin (NG), as the main component of gunpowder formula, has been widely used in national defense and mining blasting operations. At the same time, it is used in various propellant formulas as an important energetic plasticizer component. One of the most widely used energetic materials. However, due to its high energy and high sensitivity, it is very prone to explosion accidents under slight external stimulation, and countless safety accidents have been caused in production and application. Among the factors affecting the stability, compatibility and sensitivity of nitroglycerin, one of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/084
Inventor 刘可王民昌徐敏陈智群邓重清谢五喜张丽涵赵嘉静张皋常海
Owner XIAN MODERN CHEM RES INST
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