A method for determining the moisture content of 1,5-diazido-3-nitro-3-azopentane by proton nuclear magnetic resonance

A proton nuclear magnetic resonance spectroscopy and diazide-based technology, which is applied in the fields of nuclear magnetic resonance analysis, material analysis through resonance, and measurement devices, can solve the limitations of simple and rapid testing requirements, high cost of quantitative analysis work, and cumbersome methods and other problems, to achieve the effect of solving sensitive and explosive, simple and rapid testing, 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 method for determining the moisture content of 1,5-diazido-3-nitro-3-azopentane by proton nuclear magnetic resonance
  • A method for determining the moisture content of 1,5-diazido-3-nitro-3-azopentane by proton nuclear magnetic resonance
  • A method for determining the moisture content of 1,5-diazido-3-nitro-3-azopentane by proton nuclear magnetic resonance

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Experimental program
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Embodiment 1

[0030] 1,5-diazido-3-nitro-3-azopentane 1 Establishment of HNMR 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%); 1,5-diazido-3-nitro-3-azopentane (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 HNMR test. After the test is over, remove the NMR sample tube that has completed the test, add 20 mg of 1,5-diazido-3-nitro-3-azopentane...

Embodiment 2

[0050] Determination of Water Content in Different Batches of 1,5-diazido-3-nitro-3-azopentane by 1H NMR

[0051] Accurately weigh 10 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 samples 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 128 times, delay time 40s. Then remove the NMR sample tube after the test, add 20 mg of 1,5-diazido-3-nitro-3-azopentane, mix well, seal it 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 1,5-diazido-3-nitro-3-azopentane 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 content of 1,5-diazido-3-nitro-3-azopentane (DIANP) by proton nuclear magnetic resonance spectroscopy, which is based on the internal standard method of proton nuclear magnetic resonance to realize the detection of trace moisture The specific steps include: (1) configuration and proton nuclear magnetic resonance spectrum detection of internal standard substance sample solution; (2) 1,5-diazido-3-nitro-3-azapentyl to be measured (3) assign each characteristic peak in the hydrogen nuclear magnetic resonance spectrum, determine the characteristic peak of water and the characteristic peak of the internal standard substance, and integrate respectively, and substitute into the relevant formula to calculate the corresponding moisture content content. The method has the advantages of simple operation, small sample amount, and good repeatability, and can quickly and quantitatively detect the moisture content of 1,5-diazido-3-nitro-3-azopentane, which can be targeted Solve the key issues 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 water content of 1,5-diazido-3-nitro-3-azopentane (DIANP) by hydrogen nuclear magnetic resonance spectroscopy, which belongs to explosives Product analysis and testing field. Background technique [0002] 1,5-diazido-3-nitro-3-azopentane (DIANP), as an azide energetic plasticizer, has high energy, high burning rate, low burning temperature, and large gas production. Due to its small molecular weight, it is widely used in the fields of propellants, pyrotechnic agents, gas generating agents, and high-energy and low-ablation propellants. Due to the diffusion of moisture in the atmosphere and the non-drying of raw materials, the produced 1,5-diazido-3-nitro-3-azopentane usually contains a certain amount of water, and its content is stability, An important factor for important physical and chemical properties such as compatib...

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赵嘉静陈智群张皋常海
Owner XIAN MODERN CHEM RES INST
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