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
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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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