CN109030536A - A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate and nitroglycerine naked nitric acid ester moisture content - Google Patents
A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate and nitroglycerine naked nitric acid ester moisture content Download PDFInfo
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- CN109030536A CN109030536A CN201811249883.4A CN201811249883A CN109030536A CN 109030536 A CN109030536 A CN 109030536A CN 201811249883 A CN201811249883 A CN 201811249883A CN 109030536 A CN109030536 A CN 109030536A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/084—Detection of potentially hazardous samples, e.g. toxic samples, explosives, drugs, firearms, weapons
Abstract
The invention discloses a kind of methods for measuring a kind of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) naked nitric acid ester moisture content, realize that the quantitative detection to micro-moisture, specific steps include: the configuration and nuclear magnetic resonance spectroscopy detection of (1) internal standard compound sample solution based on nucleus magnetic hydrogen spectrum internal standard method；(2) addition of naked nitric acid ester sample to be measured and nuclear magnetic resonance spectroscopy detection；(3) characteristic peak each in nuclear magnetic resonance spectroscopy is belonged to, determines the characteristic peak and internal standard compound characteristic peak of water, and integrated respectively, substitute into the content that correlation formula calculates corresponding moisture.This method has many advantages, such as that easy to operate, sample size is few, reproducible, can quickly in triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) naked nitric acid ester contained humidity content carry out quantitative detection, can specific aim solve explosive wastewater application in correlated quality product control critical issue.
Description
Technical field
The invention belongs to energetic material gauge check fields, and in particular to a kind of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitro
The method of acid esters (TEGDN) and nitroglycerine (NG) naked nitric acid ester moisture content belongs to explosive wastewater product analysis detection field.
Background technique
Nitrate is as excellent plasticizer, and since its oxygen balance is preferable, burning and explosion property are good, answers extensively at present
For double base propellant and composite propellant field.It is both a kind of good plasticizer and propellant group of nitrocellulose
Primary energy content in, becoming to semi-rigid nitrocellulose, which can extrude molding material and reduce glass transition temperature, weight
It acts on, is indispensable important component in propellant.Especially triethylene glycol dinitrate (TEGDN) and nitroglycerine
(NG) in the form of naked nitric acid ester, since its is cheap, glass transition temperature is low, cryogenic mechanics performance is good and basic components
The low equal excellent performances of burn rate, are widely applied as the energetic plasticiser in high-energy propellant of new generation.
Due to atmosphere moisture diffusion and raw material are not dry etc., the TEGDN/NG naked nitric acid ester that produces
In usually in contain a certain amount of moisture, and the moisture content in naked nitric acid ester is to the important materialization such as its stability, compatibility
Characteristic has extreme influence.Some researches show that contain under same period of storage by the high performance bond of matrix of naked nitric acid ester
Water is bigger, and stability is lower.It being required in the operating specification of certain class composite explosives, moisture content must not be higher than 0.5%,
Therefore in actual production and storage process, strict control wherein moisture content is needed, realization contains moisture in naked nitric acid ester
The accurate detection of amount.Common trace water content has oven drying method, condensed steam water, Karl_Fischer method, near infrared spectroscopy
Deng, but due to characteristic (the nitroglycerine friction of TEGDN/NG naked nitric acid ester this system high-energy, high sensitivity, high risk
Sensitivity is 100%), to have specific demand for moisture detecting method: (1) amount of samples should be lacked as far as possible, be detected with reducing
Security risk in journey, traditional oven drying method and drier for this point, although once being applied to nitrify as standard method sweet
The detection of oil product moisture, but as macro-analysis method (test is with sample amount generally in 5~10g), it is clear that due to sample size mistake
To take greatly, there are biggish security risks for test process；(2) external force such as friction, electrostatic should be avoided in test process as far as possible
Effect is exploded under outside energy effect to avoid high sensitivity nitrate.Common karl Fischer moisture measurement method is due to test
It needs to generate electric current in the process and iodine is ionized into iodide ion, and reaction process is monitored by electricity, inevitable electric current
With the generation of charge during the test, it is clear that exist using limitation；(3) test method should be simple, convenient and rapid as far as possible, and have compared with
It is highly sensitive.For near infrared spectroscopy as relative measurement method, measurement sensitivity is higher, but its calibration needs one-to-one standard
Substance, and corresponding working curve is drawn, also higher cost, method are cumbersome for corresponding quantitative analysis work, for simple, convenient and rapid
Testing requirement there is also limitations.(4) other additives and reagent and environment item should be avoided or excluded as far as possible in test process
Influence of the moisture to measurement result in part.Quantitative nuclear magnetic resonance (Quantitative nuclear magnetic
Resonance, qNMR) technology do not need determinand reference substance, and sample pre-treatments step is easy, quick, can significantly improve inspection
Efficiency is surveyed, is included in succession by United States Pharmacopeia, British Pharmacopoeia, European Pharmacopoeia, Chinese Pharmacopoeia (2010 editions) in recent years.In recent years, by
In1H nmr quantitative sensitivity is high, qNMR technology using more and more extensive, in bulk pharmaceutical chemicals, pharmaceutical preparation, remnants
Solvent measurement, sample component ratio measuring etc. are widely used.
Summary of the invention
For the demand at this stage to explosive wastewater content accurate quantitative analysis, the present invention provides a kind of nuclear magnetic resonance spectroscopies
The method for measuring the moisture content of triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) naked nitric acid ester, this method are adopted
Accurate quantitative analysis is carried out to moisture content with nuclear magnetic resonance spectroscopy internal standard method, has that easy to operate, sampling quantity is few, reproducible etc. excellent
Point.Technical solution is specific as follows:
(1) it accurately weighs internal standard compound 5-15mg (being accurate to 0.1mg), deuterated solvent 0.5-0.8ml dissolution is added, is transferred to
In nuclear magnetic tube, membrana oralis sealing is sealed up.Prepared sample solution is placed in ultrasonic oscillation instrument and shakes 10-20s, later to sample
Product carry out nuclear magnetic resonance spectroscopy test.The quantitative nuclear-magnetism test condition are as follows: nmr spectrometer resonant frequency be 400~
800MHz, 20-35 DEG C of temperature, delay time 20s-50s, pulse angle is 30~90 °, and sampling number is 32-128 times.
(2) the nuclear-magnetism sample cell that test is completed is removed, naked nitric acid ester 10-30mg is added, then seal up membrana oralis sealing, and
It is shaken with ultrasonic oscillation instrument to uniformly mixed.Nuclear magnetic resonance spectroscopy survey is carried out again to the sample after addition naked nitric acid ester
Examination, the quantitative nuclear-magnetism test condition are consistent with previous step.
(3) after testing, the characteristic peak tested in the nuclear magnetic resonance spectroscopy obtained respectively twice is belonged to, is determined
The characteristic peak and internal standard compound characteristic peak of water, and integrate respectively, integration method is to remove after the leveling of spectrogram baseline to characteristic peak13C
It is integrated after satellites, calculates 3 times and be averaged.Water characteristic peak integral area and internal standard compound characteristic peak integral area are respectively obtained,
Data substitution formula (a) is obtained into corresponding impurity content.
In formula:
PxBiodiversity percentage composition, is indicated in-sample to be tested with %；
PSThe Reinheitszahl of-internal standard compound, is indicated with %；
msThe quality of-the internal standard compound being added, unit mg；
Quality, unit mg is added in m-naked nitric acid ester sample；
MsThe relative molecular mass of-internal standard compound；
MxThe relative molecular mass of-water；
HsThe number of resonant nucleus in the functional group of -1 mole of internal standard compound characteristic signal；
Hx- 1 mole of water generates the number of resonant nucleus in the functional group of signal；
AsThe peak area at-internal standard compound characteristic signal peak；
A1- be not added naked nitric acid ester sample water characteristic signal peak peak area；
A2The peak area at the water characteristic signal peak of the sample of-addition naked nitric acid ester；
Preferably, moisture content detection method in above-mentioned test TEGDN/NG naked nitric acid ester sample, in the step (1)
Internal standard compound is benzene, paracide, to difluorobenzene high sterling or standard substance, and deuterated solvent is deuterated dimethyl sulfoxide (DMSO).
Benzene and paracide not with naked nitric acid ester component reaction, favorable solubility, and are easier to obtain high sterling or purity rubric
Substance, all hydrogen is in identical chemical environment in substance, i.e., all there was only one group of characteristic peak in nuclear magnetic resonance spectroscopy spectrogram, fits
The internal standard compound requirement of nucleus magnetic hydrogen spectrum is quantified for this system.The selection of deuterated solvent is mainly according to the solvent of internal standard compound and sample
Property, the solvent borne of comprehensive TEGDN/NG naked nitric acid ester, benzene and toluene, can be selected deuterated acetone or deuterated dimethyl sulfoxide is molten
Agent, but in an experiment discovery sample size is close and water content it is similar under the conditions of, water peak is peak shape in deuterated DMSO solvent samples
Sharp and symmetrical single absorption peak, water characteristic peak is asymmetric bimodal in deuterated acetone solvent samples, and analysis is due to deuterated
Hydrogen atom can generate fast exchange, i.e. the hydrone content liter that a hydrogen atom is replaced by D-atom in D-atom and water in acetone
Height eventually leads to water peak in nuclear magnetic spectrogram and has occurred and splits point.It is symmetrically unimodal to compare when carrying out nuclear-magnetism characteristic peak integral calculation
Under can generate smaller integral calculation error.Consider that the effumability of acetone may be to sample nuclear magnetic spectrogram stability simultaneously
It has an impact, comprehensive analysis considers the solvent body for selecting deuterated dimethyl sulfoxide to quantify nuclear-magnetism detection as naked nitric acid ester system
It is
Preferably, TEGDN/NG naked nitric acid ester sample weighting amount should be 2-3 times of internal standard compound in experiment.The control of this condition
It is since in the test of quantitative nuclear-magnetism, one important condition is that the ratio between the two characteristic peak integrated area values contrasted are not answered
It is excessive to differ multiple, in 1:10 between 10:1, quantitative integration brings final result for discovery control in specific practical operation
Error it is smaller.Therefore comprehensively consider the factors such as moisture content, internal standard compound molecular weight in TEGDN/NG naked nitric acid ester sample, really
Determining TEGDN/NG naked nitric acid ester sample weighting amount should be 2-3 times of internal standard compound this condition, may make internal standard compound characteristic peak and water peak
Area ratio controls in the above range, detects basis as suitable quantitative nuclear-magnetism.
Since determination of moisture compares with the measurement of other impurities with particularity, i.e. either deuterated solvent, interior
There is the presence of micro-moisture in mark object or air, it is therefore necessary to exclude water contained in these parts during the test
It measures, the content of micro-moisture in Accurate Determining naked nitric acid ester sample.Integral difference assay is taken to carry out sample with regard to the design of this problem
The accurate calculating of moisture content in product only adds internal standard compound sample to naked nitric acid ester is not added first in deuterated solvent
Quantitative nuclear-magnetism detection is carried out, obtains integrated area value of the water peak relative to internal standard compound characteristic peak in this system, then try to nuclear-magnetism
It is precisely weighed in sample and naked nitric acid ester sample is added, quantitative nuclear-magnetism detection is then carried out with same experiment condition, is further obtained
Obtain integrated area value of the water peak relative to internal standard compound in this system.The mechanism tested by quantitative nuclear-magnetism, feature in nuclear magnetic spectrogram
Although the integral area at peak simultaneously not absolute terms does not have comparativity theoretically, by institute in testing twice in not cospectral graph
The internal standard compound magnitude contained is constant, and test condition is identical, therefore internal standard peak peak height, peak under conditions of instrument test is in stable condition
Shape and peak position remain unchanged, in value added and naked nitric acid ester of the water peak relative to the integrated area value of internal standard compound characteristic peak
Contained moisture magnitude is directly proportional, can be calculated by quantitative nuclear-magnetism formula.Simultaneously because the resonance frequency of nuclear magnetic resonance spectrometer
Rate is higher, i.e., power is higher, and correspondingly resolution ratio, sensitivity and sampling stability can all significantly improve.Therefore for mixing nitre
The analysis calibrating of micro-moisture, the accuracy and stabilization of the nmr spectrometer testing result of global alignment different capacity in acid esters system
Property, optimal selection 800M nmr spectrometer carries out quantitative detection, can get signal-to-noise ratio more preferably nucleus magnetic hydrogen spectrum spectrogram.
Important parameter of the delay time as quantitative nuclear-magnetism, has direct influence for the result of final quantitative integration,
Since there are multiple compounds, chemical structure is different in nuclear-magnetism sample to be measured, so that the relaxation of the proton of different protons is not
Together, it eventually leads in proton same time after the excitation of nmr spectrometer magnetic fields, it is real required for recovery Boltzmann balance
Border is different, therefore delay time is too short that may cause collected signal be not reply equilibrium state proton, and characteristic peak is caused to go out
Peak is incomplete, and quantitative result is inaccurate.By a series of pointedly to the nuclear-magnetism behavioral study of naked nitric acid ester system, repeatedly try
The fast and easy of accuracy that is final while considering experimental result, reproducibility and detection method is tested, it is final to determine selection
The delay time of 20s-50s, this parameter area can guarantee that internal standard compound and water all reach complete relaxation and the state that restores balance,
To guarantee on the basis of internal standard compound content to the accuracy of water and basis weight.
In the present invention TEGDN/NG naked nitric acid ester sample weighting amount be 10-30mg, although this is because improve dosing accuracy,
The demand for reducing error, configure highly concentrated solution as far as possible to reach the better signal-to-noise ratio of spectrogram, but sample solution concentration simultaneously
It is excessively high to may cause that solute Distribution in solution is uneven, and viscosity is excessive, cause spectral line broadening, while as far as possible for safety issue
Reduce naked nitric acid ester dosage.Therefore sample weighting amount is limited in 10-30mg, has not only reached preferable signal-to-noise ratio but also keeps the equal of solution
Even property and free-running property.
Compared to the prior art, above-mentioned TEGDN/NG naked nitric acid ester moisture content detection method established by the present invention
Mainly have the beneficial effect that (1) test takes sample size in milligram rank, dosage is few, effectively prevents conventional aqueous detection method
Due to macro-analysis dosage security risk caused greatly；(2) test method is lossless and substantially without external forces such as friction, electrostatic,
Solves the problems, such as high sensitivity nitrate sensitive explosive under outside energy effect；(3) test is simple, convenient and rapid, can quickly criticize
Amount is completed, experiment precision height, favorable reproducibility, has higher sensitivity, and without standard reference material or draw working curve；
(4) method combination internal standard method and integral difference assay have effectively removed other than sample in reagent residual moisture to test bring shadow
It rings.In summary, the method for the moisture content of quantitative nuclear magnetic resonance spectroscopy, is suitable for this kind of high energy of TEGDN/NG naked nitric acid ester
Amount, the analysis detection of high sensitivity and high risk sample provide for the trace moisture analysis detection of same type explosive wastewater product
The method and thinking of one fast quantification.
Detailed description of the invention
Fig. 1 is the nucleus magnetic hydrogen spectrum spectrogram of TEGDN/NG naked nitric acid ester
Specific embodiment
To make those skilled in the art carry out more preferably technical solution to technical solution of the present invention, below with reference to some tools
Technical solution of the present invention is further elaborated in body embodiment.
Embodiment 1
TEGDN/NG naked nitric acid ester1The foundation of H NMR spectra
1.1 instruments and sample
800 type NMR spectrometer with superconducting magnet of BrukerAscend (German BRUKER company)；MettlerToledo
Ten a ten thousandth balance of XP6 type (METTLER company of Switzerland)；(deuterated degree > 99.8%, U.S. CIL are public for deuterated dimethyl sulfoxide
Department)；5mm standard nuclear-magnetism sample cell (NORELL company of the U.S.)；(Tianjin metrological supervision detects scientific research to benzene purity rubric substance
Institute, lot number 0401)；TEGDN/NG naked nitric acid ester (Xi'an Inst. of Modern Chemistry, lot number 170903)
The preparation and measurement of 1.2 samples to be tested
Internal standard compound benzene standard substance 5-15mg is accurately weighed in 5mm nuclear magnetic tube, it is sub- that the deuterated dimethyl of 0.6ml is then added
Sulfone is sealed with sealed membrane after mixing, and prepared nuclear-magnetism sample is directly used in1H NMR test.After test, then
It is removed to the nuclear-magnetism sample cell for completing test, after addition naked nitric acid ester 10-30mg is sufficiently mixed, seals up membrana oralis sealing, then
By sample with the progress of same test condition1H NMR is tested, wherein test parameter and condition are as follows: observing frequency 800.3MHz, measurement
Temperature 300K, 90 ° of pulses, 3 μ s of spectrum width, sampled data points 65536, scanning times 64 times, delay time 40s.
1.3 sample1H H NMR spectroscopy map analysis
According to1H NMR spectra data in literature, the chemical property of comprehensive TEGDN/NG, using 3.5 pairs of detection institutes of Topspin
?1H NMR spectra calibrated, baseline correction and phase adjustment, divides situation and chemistry according to the coupling at proton signal peak column
Shift value is belonged to accordingly, as shown in table 1 below.The water proton signals peak and chemical shift δ of chemical shift δ 3.33
7.37 benzene proton signal peak separates well and symmetrically and evenly with other signal peaks, meets the primary condition of quantitative nuclear-magnetism.
2 TEGDN/NG naked nitric acid ester nucleus magnetic hydrogen spectrum Spectra peak recognition table of table
1.4 methodological study
Stability: taking with portion TEGDN/NG naked nitric acid ester sample, according to above-mentioned experiment condition and method, respectively 0,
2,4,6,8,12h carry out1H NMR experiment records the relative integral area of water peak to calculate the moisture relative amount of sample, meter
Calculate RSD value；
Repeatability: taking same 6 parts of batch TEGDN/NG naked nitric acid ester, carries out according to above-mentioned experiment condition and method1H
NMR experiment records the relative integral area of water peak to calculate the moisture relative amount of sample, calculates RSD value；
Precision: it takes with portion TEGDN/NG naked nitric acid ester sample, according to above-mentioned experiment condition and method METHOD FOR CONTINUOUS DETERMINATION 6
It is secondary, the relative integral area of water peak is recorded to calculate the moisture relative amount of sample, calculates RSD value；
Recovery of standard addition: taking same batch TEGDN/NG naked nitric acid ester sample, according to above-mentioned experiment condition and method into
Row1After H NMR experiment, then accurate that 3mg is added, 5mg pure water is carried out according to above method after pure water is added every time1H NMR
Experiment records the relative integral area of water peak to calculate moisture relative amount, calculates the rate of recovery.
Linear verification: taking same batch TEGDN/NG naked nitric acid ester sample, and precision weighs sample about 10mg, 20mg,
30mg, 40mg carry out 1H NMR experiment according to above-mentioned experiment condition and method respectively, record the relative integral area of water peak to
Calculate moisture relative amount, statistical test result it is linear.
Experimental result is shown in the following table 2, statistics indicate that method has good linear relationship, precision, stability and repetition
Property, while recovery of standard addition value shows method equally and has preferable accuracy.
2 nuclear magnetic resonance hydrogen spectruming determining TEGDN/NG naked nitric acid ester moisture methodological study result of table
Embodiment 2
Moisture content in nuclear magnetic resonance hydrogen spectruming determining different batches TEGDN/NG naked nitric acid ester
Internal standard compound benzene 5.3mg is accurately weighed in 5mm nuclear magnetic tube, 0.6ml deuterated dimethyl sulfoxide is then added, mixing is equal
It is sealed after even with sealed membrane, prepared nuclear-magnetism sample is directly used in1H NMR test, test parameter and condition are as follows: observation frequency
Rate 800.3MHz, measuring temperature 300K, 90 ° of pulses, 3 μ s of spectrum width, sampled data points 65536, scanning times 128 times, when delay
Between 30s.The nuclear-magnetism sample cell that test is completed is removed again, after addition naked nitric acid ester 15mg is sufficiently mixed, seals up membrana oralis sealing,
Again by sample with the progress of same test condition1H NMR test.The TEGDN/NG of three batches of different lot numbers is mixed by the same way
Nitrate sample is detected, and nmr spectrum is recorded, and calculates moisture content, as a result such as the following table 3.
3 different batches TEGDN/NG naked nitric acid ester determination of moisture of table
| Lot number | Water content/% |
| 180403 | 0.963 |
| 180418 | 1.032 |
| 180425 | 0.856 |
You need to add is that above-mentioned specific embodiment carried out the moisture detecting method of TEGDN/NG naked nitric acid ester
It is described as illustrative and non-limiting, above embodiments 1-2 is not the implementable whole embodiments of this patent, can be according to limited model
It encloses and specifically enumerates more examples again, therefore the modifications and variations in the case where not departing from present general inventive concept, belong to present invention protection model
Within enclosing.
The present invention establishes the nuclear magnetic resonance spectroscopy trace water content of TEGDN/NG naked nitric acid ester, solves biography
The big safety problem of detection method amount of samples of uniting is prominent, needs one-to-one standard substance, the problems such as method is cumbersome, surveys
Examination takes that sample size dosage is few, and test method is lossless and substantially without external forces such as friction, electrostatic, effectively prevents conventional aqueous
Detection method is since macro-analysis dosage is big and high sensitivity nitrate the problem of sensitive explosive, is surveyed under outside energy effect
It tries simple, convenient and rapid, can be completed with rapid batch, experiment precision is high, favorable reproducibility, in combination with internal standard method and integral difference assay,
Having effectively removed other than sample residual moisture in reagent influences test bring.Especially suitable for high-energy, high sensitivity, high-risk
Dangerous TEGDN/NG naked nitric acid ester sample detection provides effective analysis for the control of the quality of explosive wastewater raw material and product
Ways and means.
Claims (4)
1. a kind of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) naked nitric acid ester moisture
The method of content, it is characterised in that include step in detail below:
(1) 5~15mg of internal standard compound is weighed, 0.5~0.8ml of deuterated reagent dissolution is added, is transferred in nuclear magnetic tube, it is close to seal up membrana oralis
Prepared sample solution is placed in 10~20s of concussion in ultrasonic oscillation instrument, carries out nuclear magnetic resonance spectroscopy to sample later by envelope
Test, the quantitative nuclear-magnetism test condition are as follows: nmr spectrometer resonant frequency is 400~800MHz, 20~35 DEG C of temperature, is postponed
Time is 20s~50s, and pulse angle is 30~90 °, and sampling number is 32~128 times；
(2) the nuclear-magnetism sample cell that test is completed is removed, 10~30mg of naked nitric acid ester is added, then seal up membrana oralis sealing, be used in combination
The concussion of ultrasonic oscillation instrument carries out nuclear magnetic resonance spectroscopy test, institute to the sample after addition TEGDN/NG naked nitric acid ester again
The quantitative nuclear-magnetism test condition stated is consistent with previous step；
(3) after testing, the characteristic peak in nuclear magnetic resonance spectroscopy obtained respectively to step 1 and step 2 belongs to, really
Determine the characteristic peak and internal standard compound characteristic peak of water, and integrate respectively, integration method is to go after the leveling of spectrogram baseline to characteristic peak
It removes13It is integrated after C satellites, calculates 3 times and be averaged, respectively obtain water characteristic peak integral area and internal standard compound characteristic peak integral face
Data substitution following formula is obtained corresponding moisture content by product:
Wherein PxFor moisture content in sample to be tested, PSFor the Reinheitszahl of internal standard compound, msFor the quality of the internal standard compound of addition, m
Quality, M is added for naked nitric acid ester samplesFor the relative molecular mass of internal standard compound, MxFor the relative molecular mass of water, HsIt rubs for 1
The number of resonant nucleus, H in the functional group of your internal standard compound characteristic signalxResonant nucleus in the functional group of signal is generated for 1 mole of water
Number, AsFor the peak area at internal standard compound characteristic signal peak, A1For be not added naked nitric acid ester sample water characteristic signal peak peak
Area, A2For the peak area at the water characteristic signal peak of the sample of addition naked nitric acid ester.
2. nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) mixing according to claim 1
The method of nitrate moisture content, which is characterized in that deuterated solvent used is attached most importance to hydrogen dimethylamino base sulfoxide.
3. nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG) mixing according to claim 1
The method of nitrate moisture content, internal standard compound used require for the benzene of high sterling or standard items, paracide or to difluorobenzene.
4. being mixed according to claim 3 nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) and nitroglycerine (NG)
The method of nitrate moisture content, which is characterized in that TEGDN/NG naked nitric acid ester sample-adding quality should be 2-3 times of internal standard compound.
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