CN109030539B - Method for measuring moisture content of 1, 5-diazido-3-nitro-3-aza pentane by nuclear magnetic resonance hydrogen spectrum - Google Patents
Method for measuring moisture content of 1, 5-diazido-3-nitro-3-aza pentane by nuclear magnetic resonance hydrogen spectrum Download PDFInfo
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Abstract
The invention discloses a method for measuring the moisture content of 1, 5-diazido-3-nitro-3-aza pentane (DIANP) by nuclear magnetic resonance hydrogen spectrum, which realizes the quantitative detection of trace moisture based on a nuclear magnetic hydrogen spectrum internal standard method and comprises the following specific steps: (1) preparing an internal standard substance sample solution and detecting a nuclear magnetic resonance hydrogen spectrum; (2) adding a 1, 5-diazido-3-nitro-3-aza pentane sample to be detected and detecting a nuclear magnetic resonance hydrogen spectrum; (3) attributing each characteristic peak in the nuclear magnetic resonance hydrogen spectrum, determining the characteristic peak of water and the characteristic peak of an internal standard substance, respectively integrating, and substituting into a correlation formula to calculate the corresponding water content. The method has the advantages of simple and convenient operation, small sample amount, good repeatability and the like, can quickly carry out quantitative detection on the water content of the 1, 5-diazido-3-nitro-3-aza-pentane, and can pertinently solve the key problem of related quality control in the application of explosives and powders.
Description
Technical Field
The invention belongs to the field of measurement and detection of energetic materials, and particularly relates to a method for measuring the water content of 1, 5-diazido-3-nitro-3-aza-pentane (DIANP) by using nuclear magnetic resonance hydrogen spectrometry, belonging to the field of analysis and detection of explosives and powders products.
Background
1, 5-diazido-3-nitryl-3-aza pentane (DIANP) is used as nitrine energetic plasticizer, has the characteristics of high energy, high burning speed, low burning temperature, large gas production rate, low relative molecular weight of first-grade fuel gas and the like, and is widely applied to the fields of propellant, pyrotechnic agent, gas generating agent, high-energy low-ablation propellant and the like at present. The 1, 5-diazido-3-nitro-3-aza pentane produced usually contains a certain amount of water due to the diffusion of water in the atmosphere and the non-drying of raw materials, and the content of the water is an important factor of important physicochemical properties such as stability, compatibility and the like. The requirement of the use specification of certain mixed explosives is that the moisture content is not higher than 0.5 percent, so that the moisture content in the mixed explosives needs to be strictly controlled in the actual production and storage processes, and the moisture content in the 1, 5-diazido-3-nitro-3-aza-pentane can be accurately detected. Common trace moisture detection methods include a drying method, a dryer method, a karl fischer method, a near infrared spectroscopy method, and the like, but due to the characteristics of high energy, high sensitivity, and high risk of 1, 5-diazido-3-nitro-3-azapentane as a azide compound, there is a specific demand for a moisture detection method: (1) the sample taking amount is required to be as small as possible so as to reduce potential safety hazards in the detection process. Although the traditional drying method and dryer are used as a standard method for detecting the moisture of explosive products, the traditional drying method and dryer are used as a constant analysis method (the sample amount for testing is generally 5-10 g), obviously, the sample amount is too large, so that great potential safety hazards exist in the taking and testing process; (2) in the test process, external force effects such as friction, static electricity, impact and the like are avoided as much as possible so as to avoid combustion and explosion of the high-sensitivity azide under the action of external energy. In a common Karl Fischer moisture test method, current is required to be generated in the test process to ionize iodine into iodine ions, and the reaction process is monitored through electric quantity, so that the generation of current and charge in the test process cannot be avoided, and obviously, the use limitation exists; (3) the test method should be as simple and rapid as possible and have high sensitivity. The near infrared spectroscopy is used as a relative measurement method, the test sensitivity is high, but calibration of the near infrared spectroscopy needs standard substances in one-to-one correspondence, corresponding working curves are drawn, corresponding quantitative analysis work is high in cost and complex in method, and the requirement for simple and rapid test is limited. (4) Other additives and reagents and the influence of moisture in environmental conditions on the measurement result should be avoided or excluded as much as possible in the test process. The Quantitative nuclear magnetic resonance (qNMR) technology does not need a reference substance of an object to be detected, the sample pretreatment step is simple and quick, the detection efficiency can be obviously improved, and the Quantitative nuclear magnetic resonance (qNMR) technology is successively recorded and recorded by United states pharmacopoeia, British pharmacopoeia, European pharmacopoeia and Chinese pharmacopoeia (2010 edition) in recent years. In recent years, due to the high sensitivity of the hydrogen nuclear magnetic resonance spectroscopy quantitative technology, the application of the qNMR technology is more and more extensive, and the method is widely applied to the aspects of bulk drugs, pharmaceutical preparations, residual solvent determination, sample component ratio determination and the like.
Disclosure of Invention
Aiming at the requirement of accurate quantification of the explosive and powder content at the present stage, the invention provides a method for measuring the moisture content of 1, 5-diazido-3-nitro-3-aza pentane (DIANP) by a nuclear magnetic resonance hydrogen spectrum. The technical scheme is as follows:
(1) accurately weighing 5-15 mg of internal standard substance, adding 0.5-0.8 ml of deuterated solvent for dissolving, transferring into a nuclear magnetic tube, and sealing with a sealing film. And placing the prepared sample solution in an ultrasonic oscillator, oscillating and uniformly mixing, and then carrying out nuclear magnetic resonance hydrogen spectrum test on the sample. The quantitative nuclear magnetic test conditions are as follows: the resonance frequency of a nuclear magnetic spectrometer is 400-800 MHz, the temperature is 20-35 ℃, the delay time is 30-60 s, the pulse angle is 30-90 degrees, and the sampling frequency is 32-128 times.
(2) And taking down the tested nuclear magnetic sample tube, adding 20-40mg of 1, 5-diazido-3-nitro-3-aza pentane, adding a sealing film for sealing, and vibrating by using an ultrasonic vibrator until the mixture is uniformly mixed. And (3) performing the nuclear magnetic resonance hydrogen spectrum test again on the sample added with the 1, 5-diazido-3-nitro-3-aza-pentane, wherein the quantitative nuclear magnetic test condition is consistent with that in the previous step.
(3) After the test is finished, attributing characteristic peaks in the nuclear magnetic resonance hydrogen spectrums respectively obtained by the two tests, determining the characteristic peak of water and the characteristic peak of an internal standard substance, respectively integrating, wherein the integration method comprises the steps of leveling a spectrogram base line, and removing the characteristic peaks13And C, integrating after the satellite peak, and calculating 3 times to obtain an average value. And (3) respectively obtaining the integral area of the characteristic peak of the water and the integral area of the characteristic peak of the internal standard substance, and substituting the data into the formula (a) to obtain the corresponding impurity content.
In the formula:
Px-the mass percentage of moisture in the sample to be tested, expressed in%;
PS-the value of the purity of the internal standard, expressed in%;
ms-mass of added internal standard in mg;
adding m-1, 5-diazido-3-nitryl-3-aza pentane sample with mass of unit mg;
Ms-relative molecular mass of internal standard;
Mx-the relative molecular mass of water;
Hs-1 mole of the number of resonating nuclei on the functional group of the internal standard signature;
Hx-the number of resonant nuclei on 1 mole of water-signaling functional group;
As-peak area of the internal standard characteristic signal peak;
A1peak area of the water characteristic signal peak of the sample without 1, 5-diazido-3-nitro-3-aza pentane added;
A2adding the peak area of the water characteristic signal peak of the 1, 5-diazido-3-nitro-3-aza-pentane sample;
preferably, in the method for detecting the moisture content in the sample tested for 1, 5-diazido-3-nitro-3-aza pentane, in the step (1), the internal standard substance is hexamethyldisiloxane, benzene and 1,1,2, 2-tetrachloroethane high-purity product or standard substance, and the deuterated solvent is deuterated dimethyl sulfoxide (DMSO). The hexamethyldisiloxane, the benzene and the 1,1,2, 2-tetrachloroethane do not react with the 1, 5-diazido-3-nitro-3-aza pentane component, the dissolubility is good, a high-purity product or a purity standard substance can be easily obtained, all hydrogen in the substance is in the same chemical environment, namely, only one group of characteristic peaks exist in a nuclear magnetic resonance hydrogen spectrum, and the hexamethyldisiloxane, the benzene and the 1,1,2, 2-tetrachloroethane are suitable for the internal standard substance requirement of the quantitative nuclear magnetic hydrogen spectrum of the body system. The selection of the deuterated solvent is mainly based on the solvent properties of an internal standard substance and a sample, and the solvent properties of 1, 5-diazido-3-nitro-3-aza-pentane and the internal standard substance are integrated, and deuterated acetone or deuterated dimethyl sulfoxide can be selected as the solvent, but in the experiment, under the conditions that the sample amount is close and the water content is close, the water peak in the deuterated DMSO solvent sample is a single absorption peak with a sharp and symmetrical peak shape, the characteristic peak in the deuterated acetone solvent sample is an asymmetrical double peak, and the analysis is that the deuterium atom in the deuterated acetone and the hydrogen atom in water can generate rapid exchange, namely the content of the water molecule with one hydrogen atom substituted by the deuterium atom is increased, and finally the water peak in a nuclear magnetic spectrum is split. When nuclear magnetism characteristic peak integral calculation is carried out, symmetrical single peak generates smaller integral calculation error compared with the single peak. Meanwhile, considering that the volatility of acetone may influence the stability of a nuclear magnetic spectrogram of a sample, and comprehensively analyzing and considering that deuterated dimethyl sulfoxide is selected as a solvent system for quantitative nuclear magnetic detection of a 1, 5-diazido-3-nitro-3-aza-pentane system.
Preferably, the amount of 1, 5-diazido-3-nitro-3-aza pentane weighed in the experiment should be 1-3 times that of the internal standard. The control of the condition is because an important condition in the quantitative nuclear magnetic test is that the ratio of the integral area values of two compared characteristic peaks does not differ by a multiple too much, and the control is found in the specific practical operation to be between 1:10 and 10:1, and the error of the quantitative integration on the final result is small. Therefore, the conditions that the sample weighing amount of the 1, 5-diazido-3-nitro-3-aza pentane is 1-3 times that of the internal standard substance are determined by comprehensively considering the factors such as the water content in the 1, 5-diazido-3-nitro-3-aza pentane sample, the molecular weight of the internal standard substance and the like, so that the ratio of the characteristic peak area and the water peak area of the internal standard substance can be controlled in the above range, and the quantitative nuclear magnetic detection method is suitable as the basis.
Because the water content determination has the particularity compared with the determination of other impurities, namely, the existence of trace water in the deuterated solvent, the internal standard substance or the air, the water contained in the parts is removed in the testing process, and the trace water content in the 1, 5-diazido-3-nitro-3-aza-pentane sample is accurately determined. The method is characterized in that an integral difference method is adopted to accurately calculate the water content in a sample, namely, an internal standard sample is only added into a deuterated solvent without adding 1, 5-diazido-3-nitro-3-aza pentane to carry out quantitative nuclear magnetic detection to obtain the integral area value of a water peak in the system relative to the characteristic peak of the internal standard, then a 1, 5-diazido-3-nitro-3-aza pentane sample is accurately weighed and added into the nuclear magnetic sample, and then quantitative nuclear magnetic detection is carried out under the same experimental conditions to further obtain the integral area value of the water peak in the system relative to the internal standard. By the mechanism of quantitative nuclear magnetic test, although the integral area of the characteristic peak in the nuclear magnetic spectrogram is not an absolute value and theoretically has no comparability in different spectrograms, because the internal standard substance values contained in two tests are unchanged and the test conditions are the same, the peak height, the peak shape and the peak position of the internal standard substance are all kept unchanged under the condition that the instrument test state is stable, the integral area value of the water peak relative to the characteristic peak of the internal standard substance is increased in proportion to the water content value contained in the 1, 5-diazido-3-nitro-3-aza pentane, and the calculation can be carried out through a quantitative nuclear magnetic formula. Meanwhile, the higher the resonance frequency of the nuclear magnetic resonance spectrometer, namely the higher the power, the resolution, the sensitivity and the sampling stability are obviously improved correspondingly. Therefore, for the analysis and verification of trace moisture in the 1, 5-diazido-3-nitro-3-aza-pentane system, the accuracy and stability of the detection result of the nuclear magnetic spectrometer with different powers are comprehensively compared, and the nuclear magnetic hydrogen spectrum with better signal-to-noise ratio can be obtained by optimally selecting the 800M nuclear magnetic spectrometer for quantitative detection.
The delay time is used as an important parameter of quantitative nuclear magnetism, the final quantitative integration result is directly influenced, and due to the fact that various compounds exist in a nuclear magnetism sample to be detected, chemical structures are different, the relaxation of protons of different protons is different, and finally the fact that Boltzmann balance needs to be recovered is different after the protons are excited under the action of a magnetic field of a nuclear magnetism spectrometer within the same time, so that the acquired signals are protons in an unreturned equilibrium state due to the fact that the delay time is too short, the characteristic peak is incomplete, and the quantitative result is inaccurate. Through a series of nuclear magnetic behavior researches on a targeted 1, 5-diazido-3-nitro-3-aza-pentane system, accuracy and reproducibility of an experimental result and convenience and rapidness of a detection method are considered in multiple tests, delay time of 30s-60s is determined and selected finally, and the parameter range can ensure that an internal standard substance and water can be completely relaxed and an equilibrium state is recovered, so that the accuracy of water quantification by taking the content of the internal standard substance as a reference is ensured.
In the invention, the sample weighing amount of the 1, 5-diazido-3-nitro-3-aza-pentane is 20-40mg, because although the requirements of improving the quantitative accuracy and reducing the error are met, a high-concentration solution is prepared as much as possible to achieve a better signal-to-noise ratio of a spectrogram, the concentration of the sample solution is too high, the solute distribution in the solution is uneven, the viscosity is too high, the spectral line is widened, and the dosage of the 1, 5-diazido-3-nitro-3-aza-pentane is reduced as much as possible due to the safety problem. Therefore, the sample weighing is limited to 20-40mg, and the better signal-to-noise ratio is achieved while the uniformity and the fluidity of the solution are kept.
Compared with the prior art, the method for detecting the moisture content of the 1, 5-diazido-3-nitro-3-aza pentane, which is established by the invention, has the main beneficial effects that: (1) the amount of the sample to be taken in the test is small, so that the potential safety hazard caused by large sample taking amount in the traditional moisture detection method is effectively avoided; (2) the test method basically has no external force action such as friction, static electricity and the like, is used for nondestructive testing, and solves the problem that the high-sensitivity azide is sensitive and easy to explode under the action of external energy; (3) the method has the advantages of simple and rapid test, rapid batch completion, high experimental precision, good reproducibility, high sensitivity, and no need of standard reference substance or working curve drawing; (4) the method combines an internal standard method and an integral difference method, and effectively removes the influence of residual moisture in reagents except the sample on the test. The method for quantifying the moisture content of the nuclear magnetic resonance hydrogen spectrum is suitable for analyzing and detecting azide samples with high energy, high sensitivity and high risk, such as 1, 5-diazide-3-nitro-3-aza-pentane, and provides a rapid quantitative method and thought for analyzing and detecting trace moisture of the same type of explosive products.
Drawings
FIG. 1 is a nuclear magnetic hydrogen spectrum of 1, 5-diazido-3-nitro-3-aza pentane
FIG. 2 shows the chemical structure of 1, 5-diazido-3-nitro-3-aza pentane
Detailed Description
In order to make the technical solutions of the present invention better for those skilled in the art, the technical solutions of the present invention are further described in detail below with reference to some specific embodiments.
Example 1
1, 5-diazido-3-nitro-3-azapentane1Establishment of HNMR atlas
1.1 Instrument and sample
Bruker Ascend 800 superconducting nuclear magnetic resonance spectrometer (Bruker, germany); a one-hundred-thousandth balance model Mettler Toledo XP6 (Mettler corporation, switzerland); deuterated dimethyl sulfoxide (deuteration > 99.8%, CIL corporation, USA); 5mm standard nuclear magnetic sample tubes (NORELL, USA); hexamethyldisiloxane high purity (Annaiji chemistry, purity 99%); 1, 5-diazido-3-nitro-3-azapentane (Seisan institute of recent chemistry).
1.2 preparation and determination of samples to be determined
Accurately weighing 15mg of internal standard hexamethyldisiloxane in a 5mm nuclear magnetic tube, adding 0.5ml of deuterated dimethyl sulfoxide, mixing uniformly, sealing with a sealing film, and directly applying the prepared nuclear magnetic sample to a 5mm nuclear magnetic tube1HNMR test. After the test is finished, taking down the nuclear magnetic sample tube after the test is finished, adding 20mg of 1, 5-diazido-3-nitro-3-aza pentane, fully mixing, sealing by a sealing membrane, and carrying out the test on the sample under the same test conditions1H NMR testing, wherein the test parameters and conditions are: frequency was observed at 800.3MHz, temperature was measured at 300K, 90 pulse, spectral width 3 μ s, data point sampled 65536, scan number 64, delay time 40 s.
1.3 samples1H NMR Spectrum analysis
According to1H NMR spectrum literature data, and by combining chemical properties of 1, 5-diazido-3-nitro-3-aza pentane and adopting Topspin 3.5 pair for detection1The H NMR spectrum is subjected to calibration, baseline correction and phase adjustment, and corresponding attribution is carried out according to the coupling column conditions and the chemical shift values of proton signal peaks, as shown in the following Table 1. The water proton signal peak with chemical shift delta 3.32 and the hexamethyldisiloxane signal peak with chemical shift delta 0.03 are well separated from other signal peaks, are symmetrical and uniform, and meet basic conditions of quantitative nuclear magnetism.
TABLE 21, 5-diazido-3-nitro-3-aza-pentane nuclear magnetic hydrogen spectrum peak attribution table
1.4 methodological considerations
Stability: the same 1, 5-diazido-3-nitro-3-aza pentane sample is taken and is respectively carried out for 0, 2, 4, 6, 8 and 12h according to the experimental conditions and the method1H NMR experiment, recording the relative integral area of water peak to calculate the relative content of water in the sample, and calculating RSD value;
repeatability: the same batch of 6 parts of 1, 5-diazido-3-nitro-3-aza pentane is taken and processed according to the experimental conditions and the method1H NMR experiment, recording the relative integral area of water peak to calculate the relative content of water in the sample, and calculating RSD value;
precision: taking the same 1, 5-diazido-3-nitryl-3-aza pentane sample, continuously measuring for 6 times according to the experimental conditions and the method, recording the relative integral area of water peak to calculate the relative moisture content of the sample, and calculating RSD value;
and (3) standard addition recovery rate: the same batch of 1, 5-diazido-3-nitro-3-aza pentane samples were taken and the experimental conditions and methods were followed1After the H NMR experiment, 2mg, 5mg of pure water were then added precisely, and each time after the addition of pure water, the procedure was followed as above1And H NMR experiments, recording the relative integral area of a water peak to calculate the relative content of water, and calculating the recovery rate.
And (3) linear verification: taking the same batch of 1, 5-diazido-3-nitro-3-aza pentane samples, precisely weighing about 20mg, 25mg, 30mg and 35mg of the samples, and respectively carrying out the following steps according to the experimental conditions and methods1And H NMR experiment, recording the relative integral area of a water peak to calculate the relative content of the water, and counting the linearity of the test result.
The experimental results are shown in table 2 below, and data show that the method has good linear relationship, precision, stability and repeatability, and the benchmarking recovery rate value shows that the method also has good accuracy.
TABLE 2 NMR Hydrogen Spectroscopy for determination of 1, 5-diazido-3-nitro-3-azapentane moisture methodological findings
Example 2
Nuclear magnetic resonance hydrogen spectrum determination of water content in different batches of 1, 5-diazido-3-nitro-3-aza pentane
Accurately weighing 10mg of internal standard substance hexamethyldisiloxane in a 5mm nuclear magnetic tube, adding 0.6ml of deuterated dimethyl sulfoxide, mixing uniformly, sealing with a sealing film, and directly applying the prepared nuclear magnetic sample to a 5mm nuclear magnetic tube1H NMR test, the test parameters and conditions are as follows: frequency was observed at 800.3MHz, temperature was measured at 300K, 90 pulse, spectral width 3 μ s, data point sampled 65536, scan number 128, delay time 40 s. Taking down the tested nuclear magnetic sample tube, adding 20mg of 1, 5-diazido-3-nitro-3-aza pentane, mixing, sealing with sealing membrane, and testing under the same test conditions1H NMR measurement. Three batches of 1, 5-diazido-3-nitro-3-aza pentane samples of different batches were tested according to the same method, nuclear magnetic resonance spectra were recorded, and the water content was calculated, with the results shown in table 3 below.
TABLE 3 determination of the moisture content of the different batches of 1, 5-diazido-3-nitro-3-azapentane
| Batch number | Water content/% |
| 180402 | 0.593 |
| 180509 | 0.536 |
| 171113 | 0.326 |
It should be added that the above-mentioned embodiments are illustrative and not restrictive of the method for detecting moisture in 1, 5-diazido-3-nitro-3-azapentane, and the above examples 1-2 are not all examples of the present invention, and further examples are specifically mentioned according to the limited scope, so that modifications and changes without departing from the general concept of the present invention are within the scope of the present invention.
The invention establishes the nuclear magnetic resonance hydrogen spectrum trace moisture detection method of 1, 5-diazide-3-nitro-3-aza pentane, solves the problems of large sample consumption and safety, requirement of standard substances corresponding to one another, complicated operation of the method and the like of the traditional detection method, has small sample consumption for testing, is lossless in the testing method, basically has no external force action such as friction, static electricity and the like, effectively avoids the problems that the traditional moisture detection method is sensitive and explosive under the action of external energy due to large constant analysis consumption and high-sensitivity azide, is simple and rapid to test, can be rapidly completed in batches, has high experimental precision and good reproducibility, and effectively removes the influence of residual moisture in reagents except the sample on the test by combining an internal standard method and an integral difference method. The method is particularly suitable for detecting the 1, 5-diazido-3-nitro-3-aza-pentane sample with high energy, high sensitivity and high risk, and provides an effective analysis method and means for quality control of explosive raw materials and products.
Claims (4)
1. A method for measuring 1, 5-diazido-3-nitro-3-aza pentane by nuclear magnetic resonance hydrogen spectrum is characterized by comprising the following specific steps:
(1) weighing 5-15 mg of internal standard substance, adding 0.5-0.8 ml of deuterated reagent for dissolving, transferring into a nuclear magnetic tube, and sealing with a sealing film; placing the prepared sample solution in an ultrasonic oscillator, oscillating for 30-60 s, and then testing the nuclear magnetic resonance hydrogen spectrum, wherein the nuclear magnetic resonance hydrogen spectrum testing conditions are as follows: the resonance frequency of a nuclear magnetic spectrometer is 400-800 MHz, the temperature is 20-35 ℃, the delay time is 30-60 s, the pulse angle is 30-90 degrees, and the sampling frequency is 32-128 times;
(2) taking down the tested nuclear magnetic sample tube, adding 20-40mg of 1, 5-diazido-3-nitro-3-azapentane, sealing with a sealing film, vibrating with an ultrasonic oscillator, and performing nuclear magnetic resonance hydrogen spectrum test on the sample added with the 1, 5-diazido-3-nitro-3-azapentane again, wherein the quantitative nuclear magnetic test conditions are consistent with those in the previous step;
(3) after the test is finished, attributing characteristic peaks in the nuclear magnetic resonance hydrogen spectrums obtained in the first step and the second step respectively, determining the characteristic peaks of water and the characteristic peaks of an internal standard substance, and integrating the characteristic peaks respectively, wherein the integration method comprises the steps of removing the characteristic peaks after the base line of the spectrogram is leveled13And C, integrating after the satellite peak, calculating 3 times, taking an average value, respectively obtaining the water characteristic peak integral area and the internal standard substance characteristic peak integral area, and substituting the data into the following formula to obtain the corresponding water content:
wherein P isxIs the mass fraction of water in the sample to be measured, PSIs the purity value of the internal standard, msFor the mass of the added internal standard, M is the mass of the added 1, 5-diazido-3-nitro-3-aza pentane sample, MsRelative molecular mass of internal standard, MxIs the relative molecular mass of water, HsNumber of resonating nuclei on functional group which is a characteristic signal of 1 mole of internal standard, HxNumber of resonant nuclei on functional groups that produce a signal for 1 mole of water, AsIs the peak area of the characteristic signal peak of the internal standard substance, A1The peak area of the water characteristic signal peak of the sample to which 1, 5-diazido-3-nitro-3-aza-pentane had not been added, A2For adding 1, 5-diazido-3-Peak area of water characteristic signal peak of nitro-3-azapentane sample.
2. The method for measuring the moisture content of 1, 5-diazido-3-nitro-3-aza pentane according to the nuclear magnetic resonance hydrogen spectrum of claim 1, wherein the deuterated reagent is deuterium dimethyl sulfoxide.
3. The method for measuring the moisture content of 1, 5-diazido-3-nitro-3-aza pentane through nuclear magnetic resonance hydrogen spectroscopy according to claim 1, characterized in that the internal standard substance is benzene, 1,2,2, -tetrachloroethane or hexamethyldisiloxane which are high-purity or standard substances.
4. The method for measuring the moisture content of 1, 5-diazido-3-nitro-3-aza pentane according to the nuclear magnetic resonance hydrogen spectrum of claim 3, wherein the loading mass of the 1, 5-diazido-3-nitro-3-aza pentane is 1 to 3 times of that of the internal standard substance.
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