CN109239120B - Method for measuring moisture content of 1, 2-propylene glycol dinitrate by nuclear magnetic resonance hydrogen spectrum - Google Patents
Method for measuring moisture content of 1, 2-propylene glycol dinitrate 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, 2-Propylene Glycol Dinitrate (PGDN) by a 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, 2-propylene glycol dinitrate 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, 2-propylene glycol dinitrate, 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, 2-Propylene Glycol Dinitrate (PGDN) by nuclear magnetic resonance hydrogen spectrometry, belonging to the field of analysis and detection of explosives and powders products.
Background
Nitrate is used as an excellent plasticizer, and because the oxygen balance is better, the combustion and explosion performance is good, the nitrate is widely applied to the fields of composite propellants and double-base propellants at present. Particularly, 1, 2-Propylene Glycol Dinitrate (PGDN) is used as the main energy and plasticizing component in the propellant composition, plays an important role in making semi-rigid nitrocellulose into extrudable materials and reducing the vitrification temperature, and is widely applied as an energetic plasticizer in a new generation of high-energy propellant due to the excellent performances of low price, low burning rate of basic components, good low-temperature mechanical property and the like
The 1, 2-propylene glycol dinitrate obtained by production usually contains a certain amount of moisture due to the diffusion of moisture in the atmosphere and the non-drying of raw materials, and the moisture content is an important factor influencing the important physicochemical properties such as stability and compatibility of the nitrate with high energy. It has been found that the higher the water content of the nitrate-based high-energy binder, the lower the stability thereof, at the same storage time. 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 accurate detection of the moisture content in the nitrate is realized. 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 high energy, high sensitivity, and high risk characteristics of 1, 2-propanediol dinitrate as nitrate explosive, there are specific demands for moisture detection methods: (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 nitrate 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 the high-sensitivity nitrate from being combusted and exploded 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, 2-Propylene Glycol Dinitrate (PGDN) by a nuclear magnetic resonance hydrogen spectrum. The technical scheme is as follows:
(1) accurately weighing 5-15mg of internal standard substance, adding 0.5-0.8ml 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 25-35 ℃, 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 10-30mg of 1, 2-propylene glycol dinitrate, adding a sealing film for sealing, and oscillating by using an ultrasonic oscillator until the mixture is uniformly mixed. And (3) performing the nuclear magnetic resonance hydrogen spectrum test again on the sample added with the 1, 2-propylene glycol dinitrate, 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. Respectively obtaining the water characteristic peak integral area and the internal standard substance characteristic peak areaAnd (4) dividing the area, and substituting the data into a 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;
the mass of m-1, 2-propylene glycol dinitrate sample added, in 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, 2-propanediol dinitrate added;
A2-peak area of water characteristic signal peak of the sample added with 1, 2-propanediol dinitrate;
preferably, in the method for detecting the moisture content in the 1, 2-propanediol dinitrate sample, in the step (1), the internal standard substance is hexamethyldisiloxane, p-dichlorobenzene, benzene high-purity product or standard substance, and the deuterated solvent is deuterated dimethyl sulfoxide (DMSO). Benzene and p-dichlorobenzene do not react with the 1, 2-propylene glycol dinitrate component, the solubility is good, high-purity products or purity standard substances can be easily obtained, all hydrogen in the substances is in the same chemical environment, namely, a nuclear magnetic resonance hydrogen spectrum spectrogram only has one group of characteristic peaks, and the method is suitable for the internal standard substance requirement of the quantitative nuclear magnetic hydrogen spectrum of the system. The selection of the deuterated solvent is mainly based on the solvent properties of an internal standard substance and a sample, the solvent properties of the 1, 2-propylene glycol dinitrate are integrated, 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 water 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 the water can generate rapid exchange, namely, the content of the water molecule with one hydrogen atom replaced 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 spectrum 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, 2-propylene glycol dinitrate system.
Preferably, the amount of 1, 2-propanediol dinitrate weighed in the experiment should be 2-3 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 factors such as the water content in the 1, 2-propylene glycol dinitrate sample, the molecular weight of the internal standard substance and the like are comprehensively considered, the condition that the sample weighing amount of the 1, 2-propylene glycol dinitrate is 2-3 times of that of the internal standard substance is determined, the ratio of the characteristic peak area to the water peak area of the internal standard substance can be controlled in the range, and the ratio is used as a proper quantitative nuclear magnetic detection 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 content in the parts is removed in the testing process, and the content of trace water in the 1, 2-propylene glycol dinitrate 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, firstly, an internal standard sample is added into a deuterated solvent without adding 1, 2-propylene glycol dinitrate 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, the 1, 2-propylene glycol dinitrate sample is accurately weighed and added into the nuclear magnetic sample, and then, the quantitative nuclear magnetic detection is carried out under the same experimental condition 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, 2-propylene glycol dinitrate, 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, 2-propylene glycol dinitrate system, the accuracy and the 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 targeted nuclear magnetic behavior researches on a 1, 2-propylene glycol dinitrate system, the accuracy and reproducibility of experimental results and the convenience and rapidness of a detection method are considered in multiple tests, the delay time of 30s-60s is determined and selected finally, and the parameter range can ensure that the internal standard substance and water are 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, 2-propylene glycol dinitrate is 10-30mg, because although the requirements of improving the quantitative accuracy and reducing errors are met, a high-concentration solution is prepared as much as possible to achieve a better signal-to-noise ratio of a spectrogram, at the same time, the concentration of the sample solution is too high, which may cause uneven distribution of solutes in the solution and overlarge viscosity to widen a spectral line, and meanwhile, the dosage of the 1, 2-propylene glycol dinitrate is reduced as much as possible due to the safety problem. Therefore, the sample weighing is limited to 10-30mg, 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 water content of the 1, 2-propylene glycol dinitrate 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 testing 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 nitrate 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 nitrate samples with high energy, high sensitivity and high risk, such as 1, 2-propylene glycol dinitrate, and provides a rapid quantification method and thought for analyzing and detecting trace moisture of the same type of explosive and powder products.
Drawings
FIG. 1 is a nuclear magnetic hydrogen spectrum of 1, 2-propylene glycol dinitrate
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, 2-propanediolDinitrate ester1Establishment of H NMR spectra
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, 2-propanediol dinitrate (Seisan recent chemical research institute).
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 tube1H NMR measurement. After the test is finished, the nuclear magnetic sample tube which is finished is taken down, 30mg of 1, 2-propylene glycol dinitrate is added and fully mixed, a sealing film is added for sealing, and then the sample is subjected to 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 128, delay time 40 s.
1.3 samples1H NMR Spectrum analysis
According to1H NMR spectrum literature data, and by combining chemical properties of 1, 2-propanediol dinitrate 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 0.02 are well separated from other signal peaks and are symmetrical and uniform, thus meeting the basic condition of quantitative nuclear magnetism.
TABLE 11, TABLE 2-PROPYLENE DINITRATE NUCLEAR MAGNETIC HYDROGEN SPECTRUM PETROSE ACCORDING TABLE
1.4 methodological considerations
Stability: taking the same sample of 1, 2-propylene glycol dinitrate, carrying out the test at 0, 2, 4, 6, 8 and 12h according to the experimental conditions and 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: taking 6 parts of the same batch of 1, 2-propylene glycol dinitrate, and carrying out the reaction 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, 2-propylene glycol dinitrate sample, continuously measuring for 6 times according to the experimental conditions and the method, recording the relative integral area of water peaks so as to calculate the relative content of water in the sample, and calculating the RSD value;
and (3) standard addition recovery rate: taking the same batch of 1, 2-propylene glycol dinitrate sample, carrying out the test according to the experimental conditions and the method1After the H NMR experiment, 3mg, 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: and (3) taking the same batch of 1, 2-propylene glycol dinitrate samples, precisely weighing about 10mg, 12mg, 15mg and 20mg of the samples, respectively carrying out 1H NMR experiments according to the experimental conditions and the method, recording the relative integral area of water peaks to calculate the relative content of moisture, 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, 2-propanediol dinitrate moisture methodological investigation results
Example 2
Nuclear magnetic resonance hydrogen spectrum determination of water content in different batches of 1, 2-propylene glycol dinitrate
Accurately weighing 5.9mg of internal standard 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 64, delay time 40 s. Taking down the tested nuclear magnetic sample tube, adding 13mg of 1, 2-propylene glycol dinitrate, fully mixing, sealing by a sealing film, and carrying out the test on the sample under the same test conditions1H NMR measurement. Three batches of 1, 2-propylene glycol dinitrate samples of different batches were tested according to the same procedure, and the nuclear magnetic resonance spectra were recorded to calculate the water content, the results are shown in table 3 below.
TABLE 3 determination of moisture content of different batches of 1, 2-propanediol dinitrate
| Batch number | Water content/% |
| 180531 | 0.756 |
| 180320 | 0.923 |
| 180309 | 0.556 |
It should be added that the above-mentioned embodiments of the method for detecting moisture in 1, 2-propanediol dinitrate are illustrative and not restrictive, 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, 2-propylene glycol dinitrate, solves the problems of large sample consumption and safety, requirement of one-to-one corresponding standard substance, complicated operation of the method and the like of the traditional detection method, has small consumption of the sample for testing, no damage to the testing method, basically no external force action such as friction, static electricity and the like, effectively avoids the problems of large constant analysis consumption and sensitivity and easy explosion of the nitrate with high sensitivity under the action of external energy of the traditional moisture detection method, has simple and rapid test, can be quickly completed in batches, has high experimental precision and good reproducibility, and simultaneously combines an internal standard method and an integral difference method to effectively remove the influence of residual moisture in reagents except the sample on the test. The method is particularly suitable for detecting the 1, 2-propylene glycol dinitrate 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 the moisture content of 1, 2-propylene glycol dinitrate by nuclear magnetic resonance hydrogen spectrum is characterized by comprising the following specific steps:
(1) weighing 5-15mg of internal standard substance, adding 0.5-0.8ml 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 10-20 s, and then carrying out nuclear magnetic resonance hydrogen spectrum test on the sample, wherein the nuclear magnetic resonance hydrogen spectrum test conditions are as follows: the resonance frequency of a nuclear magnetic spectrometer is 400-800 MHz, the temperature is 25-35 ℃, 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 10-30mg of 1, 2-propylene glycol dinitrate, 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, 2-propylene glycol dinitrate again, wherein the quantitative nuclear magnetic test condition is consistent with that of 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, 2-propanediol dinitrate 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, 2-propanediol dinitrate was not added, A2The peak area of the water characteristic signal peak of the sample added with 1, 2-propylene glycol dinitrate was determined.
2. The method for measuring the water content of 1, 2-propanediol dinitrate according to claim 1, wherein the deuterated reagent is deuterium-depleted dimethyl sulfoxide.
3. The method for measuring the moisture content of 1, 2-propylene glycol dinitrate according to claim 1, wherein the internal standard substance used is benzene, p-dichlorobenzene or hexamethyldisiloxane which is a high purity or standard substance.
4. The method for measuring the moisture content of 1, 2-propanediol dinitrate according to claim 3, wherein the loading mass of 1, 2-propanediol dinitrate is 2-3 times that of the internal standard.
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