CN109030537B - Method for measuring water content of mixed nitrate of butanetriol trinitrate and nitroglycerin by nuclear magnetic resonance hydrogen spectroscopy - Google Patents
Method for measuring water content of mixed nitrate of butanetriol trinitrate and nitroglycerin by nuclear magnetic resonance hydrogen spectroscopy Download PDFInfo
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Abstract
The invention discloses a method for measuring the water content of mixed nitrate of butanetriol trinitrate (BTTN) and Nitroglycerin (NG) by a nuclear magnetic resonance hydrogen spectrum, which is used for realizing quantitative detection of trace water based on a nuclear magnetic hydrogen spectrum internal standard method and comprises the following specific steps of: (1) preparing an internal standard substance sample solution and detecting a nuclear magnetic resonance hydrogen spectrum; (2) adding a mixed nitrate 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 good safety, simple and convenient operation, small sample amount, good repeatability and the like, can quickly carry out quantitative detection on the water content in the mixed nitrate of the butanetriol trinitrate (BTTN) and the Nitroglycerin (NG), and aims at solving 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 moisture content of mixed nitrate of butanetriol trinitrate (BTTN) and Nitroglycerin (NG) by nuclear magnetic resonance hydrogen spectrometry, belonging to the field of analysis and detection of explosives and powders.
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 double-base propellants and composite propellants at present. The plasticizer is a good plasticizer of the nitrocellulose, is a main energy component in the composition of the propellant, plays an important role in making the semi-rigid nitrocellulose into an extrudable material and reducing the glass transition temperature, and is an indispensable important component in the propellant. In particular, in the high-energy nitrate plasticized polyether (NEPE) propellants which are currently the highest in energy level, butanetriol trinitrate (BTTN) and Nitroglycerin (NG) are used as important plasticizers in high-energy propellants and the like in the form of mixed nitrates.
Because the raw materials are not dried and the moisture in the atmosphere diffuses, the produced BTTN/NG mixed nitrate usually contains trace moisture, and the moisture content in the mixed nitrate has great influence on the stability, compatibility and other important physicochemical characteristics, and researches show that the higher the moisture content of the high-energy adhesive taking the mixed nitrate as a matrix is, the lower the stability is. The requirement in the use specification of certain mixed explosives is that the moisture content is not higher than 0.5%, so that the moisture content in the mixed explosives needs to be strictly controlled in the actual production and storage processes, such as real-time accurate detection of the moisture content in the mixed nitrate. 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 the BTTN/NG mixed nitrate system (nitroglycerin friction sensitivity is 100%), there are specific requirements for moisture detection methods: (1) the sample amount is required to be as small as possible so as to reduce the potential safety hazard in the detection process, and in this point, although the traditional drying method and the traditional dryer are used as a standard method for detecting the water content of the nitroglycerin product, the traditional drying method and the traditional 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 the great potential safety hazard exists in the taking and testing process; (2) in the test process, external force effects such as friction, static electricity and the like are avoided as much as possible so as to avoid explosion of the high-sensitivity nitrate 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 charges, so that the generation of the current and the charges in the test process cannot be avoided, and obviously, the use limitation exists; (3) the test method should be as simple as possibleFast and has 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, the reason is that1The H nuclear magnetic resonance quantitative technology has high sensitivity, and the qNMR technology is more and more widely applied, and is widely applied to the aspects of bulk drugs, pharmaceutical preparations, residual solvent determination, sample component proportion 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 mixed nitrate of butanetriol trinitrate (BTTN) and Nitroglycerin (NG) by a nuclear magnetic resonance hydrogen spectrum. The technical scheme is as follows:
(1) accurately weighing 5-10mg (accurate to 0.1mg) 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 for oscillation for 10-20s, 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 30-50 s, the pulse angle is 90 degrees, and the sampling times are 32-128 times.
(2) And taking down the tested nuclear magnetic sample tube, adding 10-30mg of mixed nitrate, adding a sealing film for sealing, and oscillating for 10-20s by using an ultrasonic oscillator until the mixture is uniformly mixed. And (3) performing the nuclear magnetic resonance hydrogen spectrum test on the sample added with the mixed nitrate again, 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;
m-mass of mixed nitrate sample added, 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 the mixed nitrate;
A2-peak area of water characteristic signal peak of sample added mixed nitrate;
preferably, in the method for detecting the moisture content in the BTTN/NG mixed nitrate sample, in the step (1), the internal standard substance is a benzene or p-dichlorobenzene high-purity product or a standard substance, and the deuterated solvent is deuterated dimethyl sulfoxide (DMSO). Benzene and p-dichlorobenzene do not react with the mixed nitrate component, the solubility 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 spectrogram, and the method is suitable for the requirement of an internal standard substance of the system quantitative nuclear magnetic hydrogen spectrum. 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 BTTN/NG mixed nitrate, benzene and toluene 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 the 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 affect 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 mixed nitrate system.
Preferably, the BTTN/NG mixed nitrate in the experiment should be weighed 2-5 times of the internal standard substance. 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 BTTN/NG mixed nitrate sample, the molecular weight of the internal standard substance and the like are comprehensively considered, the condition that the sample weighing amount of the BTTN/NG mixed nitrate is 2-5 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 can be used as a proper quantitative nuclear magnetic detection basis.
Because the water content measurement has the particularity compared with the measurement 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 test process, and the trace water content in the mixed nitrate sample is accurately measured. 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 mixed nitrate to carry out quantitative nuclear magnetic detection to obtain an integral area value of a water peak in the system relative to an internal standard characteristic peak, then, the mixed nitrate sample is accurately weighed and added into the nuclear magnetic sample, then, quantitative nuclear magnetic detection is carried out under the same experimental conditions, and the integral area value of the water peak in the system relative to the internal standard is further obtained. 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 increase value of the integral area value of the water peak relative to the characteristic peak of the internal standard substance is in direct proportion to the water content value contained in the mixed nitrate, 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 a mixed nitrate system, the accuracy and stability of detection results of nuclear magnetic spectrometers with different powers are comprehensively compared, and a nuclear magnetic hydrogen spectrum spectrogram with better signal-to-noise ratio can be obtained by selecting a 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 mixed nitrate system, the accuracy and reproducibility of experimental results and the convenience and rapidness of a detection method are considered in multiple experiments, the delay time of 30-50 s is finally determined and selected, and the parameter range can ensure that the internal standard substance and water can be completely relaxed and the 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.
The BTTN/NG mixed nitrate in the invention is weighed by 10-30mg, because although the requirements of quantitative accuracy improvement and error reduction 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 a sample solution is too high, which may cause uneven distribution of solutes in the solution and overlarge viscosity to widen the spectral line, and simultaneously, the dosage of the mixed nitrate 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 BTTN/NG mixed nitrate ester moisture content detection method has the main beneficial effects that: (1) the sample amount for testing is in milligram level, the using amount is small, and the potential safety hazard caused by large constant analysis using amount in the traditional water detection method is effectively avoided; (2) the testing method is lossless and basically has no external force action such as friction, static electricity and the like, and the problem that the high-sensitivity nitrate is sensitive and easy to explode under the action of external energy is solved; (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. By combining the above, the method for detecting the moisture content of the nuclear magnetic resonance hydrogen spectrum is suitable for analyzing and detecting high-energy, high-sensitivity and high-risk samples such as BTTN/NG mixed nitrate, 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 nuclear magnetic hydrogen spectrum of BTTN/NG mixed nitrate
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
BTTN/NG Mixed nitrate esters1Establishment of HNMR atlas
1.1 Instrument and sample
BrukerAscend 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); benzene purity standard substance (Tianjin measurement supervision and detection science institute, lot number 0401); BTTN/NG Mixed nitrate (Seisan recent chemical research institute, batch No. 180410)
1.2 preparation and determination of samples to be determined
Accurately weighing 5-15mg of internal standard substance benzene standard substance 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, the nuclear magnetic sample tube which is finished is taken down, 10-30mg of mixed nitrate is added and fully mixed, a sealing film is added for sealing, and then the sample is subjected to the same test conditions1HNMR test, wherein 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 32, delay time 30 s.
1.3 samples1HNMR spectrogram analysis
According to1HNMR spectrogram literature data, the chemical properties of BTTN/NG are integrated, and Topspin 3.5 is adopted for detection1The HNMR spectrogram 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 3.33 and the benzene proton signal peak with chemical shift delta 7.37 are well separated from other signal peaks and are symmetrical and uniform, thus meeting the basic condition of quantitative nuclear magnetism.
TABLE 1 NG/BTTN mixed nitrate nuclear magnetic hydrogen spectrum peak attribution table
1.4 methodological considerations
Stability: taking the same BTTN/NG mixed nitrate sample, and respectively carrying out the operations for 0, 2, 4, 6, 8 and 12h according to the experimental conditions and the method1HNMR experiment, recording the relative integral area of water peak to calculate the relative water content of the sample, and calculating RSD value;
repeatability: taking 6 parts of the BTTN/NG mixed nitrate ester of the same batch, and carrying out the test according to the experimental conditions and the method1HNMR experiment, recording the relative integral area of water peak to calculate the relative water content of the sample, and calculating RSD value;
precision: taking the same BTTN/NG mixed nitrate sample, continuously measuring for 6 times according to the experimental conditions and the method, recording the relative integral area of the water peak so as to calculate the relative content of the water in the sample, and calculating the RSD value;
and (3) standard addition recovery rate: taking the same batch of BTTN/NG mixed nitrate sample, and carrying out the test according to the experimental conditions and the method1After 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 (4) performing HNMR experiment, recording the relative integral area of a water peak so as to calculate the relative content of water and calculate the recovery rate.
And (3) linear verification: and (3) precisely weighing about 10mg, 20mg, 30mg and 40mg of the BTTN/NG mixed nitrate sample of the same batch, respectively carrying out 1HNMR (hydrogen sulfide magnetic resonance) experiment according to the experiment conditions and the method, recording the relative integral area of a water peak so as to calculate the relative content of 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 determination of BTTN/NG Mixed nitrate moisture methodological investigation results
Example 2
Nuclear magnetic resonance hydrogen spectrum determination of moisture content in different batches of BTTN/NG mixed nitrate
Accurately weighing 5.0mg of internal standard substance benzene into 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, 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 32, delay time 30 s. Taking down the tested nuclear magnetic sample tube, adding 10.8mg of mixed nitrate, fully mixing, sealing by a sealing film, and carrying out the same test on the sample under the same test conditions1H NMR measurement. Three batches of BTTN/NG mixed nitrate samples with different batches of numbers are detected according to the same method, nuclear magnetic resonance spectrograms are recorded, and the moisture content is calculated, wherein the results are shown in the following table 3.
TABLE 3 determination of moisture content of BTTN/NG Mixed nitrate esters in different batches
| Batch number | Water content/% |
| 180403 | 0.577 |
| 180418 | 0.766 |
| 180425 | 0.208 |
It should be added that the above-mentioned embodiments of the method for detecting moisture in a mixed nitrate of BTTN/NG are described as 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, therefore, modifications and changes without departing from the general concept of the present invention are within the protection scope of the present invention.
The invention establishes the nuclear magnetic resonance hydrogen spectrum trace moisture detection method of BTTN/NG mixed nitrate, 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 high-sensitivity nitrate under the action of external energy in 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 BTTN/NG mixed nitrate sample with high energy, high sensitivity and high danger, 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 a mixed nitrate of butanetriol trinitrate BTTN and nitroglycerin NG by nuclear magnetic resonance hydrogen spectroscopy is characterized by comprising the following specific steps:
(1) weighing 5-10mg 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 for oscillation for 10-20s, 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 20-35 ℃, the delay time is 30-50 s, the pulse angle is 90 degrees, and the sampling times are 32-128 times;
(2) taking down the tested nuclear magnetic sample tube, adding 10-30mg of mixed nitrate, adding a sealing film for sealing, oscillating for 10-20s by using an ultrasonic oscillator, and performing nuclear magnetic resonance hydrogen spectrum test on the sample added with the mixed nitrate 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 mixed nitrate sample addition, 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 without the mixed nitrate ester is A2The peak area of the water characteristic signal peak of the sample added with the mixed nitrate.
2. The method for measuring the moisture content of the mixed nitrate of the butanetriol trinitrate BTTN and the nitroglycerin NG according to the nuclear magnetic resonance hydrogen spectrum of claim 1, wherein the deuterated reagent is deuterium-enriched dimethyl sulfoxide.
3. The method for measuring the water content of the mixed nitrate of the butanetriol trinitrate BTTN and the nitroglycerin NG according to the nuclear magnetic resonance hydrogen spectrum of claim 1, wherein the used internal standard substance is benzene or p-dichlorobenzene which is a high-purity product or a standard product.
4. The method for measuring the moisture content of the mixed nitrate of the butanetriol trinitrate BTTN and the nitroglycerin NG according to the nuclear magnetic resonance hydrogen spectrum of claim 3, wherein the loading mass of the BTTN/NG mixed nitrate is 2-5 times of that of the internal standard substance.
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