CN109030535A - A kind of method of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content - Google Patents
A kind of method of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content Download PDFInfo
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Abstract
The invention discloses a kind of methods of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate (DEGDN) 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 diethylent glycol dinitrate 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 to diethylent glycol dinitrate 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 diethylene glycol dinitro
The method of acid esters (DEGDN) 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.Especially diethylent glycol dinitrate (DEGDN) is as in propellant composition
Primary energy content, to semi-rigid nitrocellulose become can extrude molding material and reduce glass transition temperature have important work
With being pushed away as high energy of new generation due to the excellent performances such as its is cheap, cryogenic mechanics performance is good and basic components burn rate is low
It is widely applied into the energetic plasticiser in agent
Due to atmosphere moisture diffusion and raw material are not dry etc., in the DEGDN that produces usually in contain
A certain amount of moisture, and the moisture content in nitrate has extreme influence to the important physicochemical characteristic such as its stability, compatibility.
Some researches show that under same period of storage, bigger as the high performance bond water content of matrix using nitrate, stability is lower.
It is required in the operating specification of certain class composite explosives, moisture content must not be higher than 0.5%, therefore in actual production and store
Cheng Zhong needs strict control wherein moisture content, realizes the accurate detection to moisture content in nitrate.Common micro-moisture
Detection method has oven drying method, condensed steam water, Karl_Fischer method, near infrared spectroscopy etc., but since DEGDN is as nitrate explosive
High-energy, high sensitivity, high risk characteristic, have specific demand for moisture detecting method: (1) the sample amount of taking should be use up
Amount is few, to reduce security risk in detection process.Traditional oven drying method and drier, although being once applied to nitre as standard method
The detection of esters of gallic acid product moisture, but as macro-analysis method (test is with sample amount generally in 5~10g), it is clear that due to sample
Measure it is excessive so that taking, there are biggish security risks for test process；(2) should be avoided as far as possible in test process friction, electrostatic,
Under outside energy effect combustion explosion occurs for the external forces such as shock to avoid high sensitivity nitrate.Common karl Fischer
Iodine is ionized into iodide ion due to needing to generate electric current in test process by moisture measurement method, and is carried out by electricity to reaction process
Monitoring, the generation of inevitable electric current and charge during the test, it is clear that exist using limitation；(3) test method should be as far as possible
It is simple, convenient and rapid, and there is higher sensitivity.For near infrared spectroscopy as relative measurement method, measurement sensitivity is higher, but it is demarcated
One-to-one standard substance is needed, and draws corresponding working curve, corresponding quantitative analysis work also higher cost, method
Cumbersome, for simple, convenient and rapid testing requirement, there is also limitations.(4) other additives should be avoided or excluded as far as possible in test process
And influence of the moisture to measurement result in reagent and environmental condition.Quantitative nuclear magnetic resonance (Quantitative nuclear
Magnetic resonance, qNMR) technology do not need determinand reference substance, and sample pre-treatments step is easy, quick, Ke Yixian
It writes and improves detection efficiency, included in succession by United States Pharmacopeia, British Pharmacopoeia, European Pharmacopoeia, Chinese Pharmacopoeia (2010 editions) in recent years.Closely
Nian Lai, since nmr quantitative sensitivity is high, qNMR technology using more and more extensive, bulk pharmaceutical chemicals, pharmaceutical preparation,
Residual 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 diethylent glycol dinitrate (DEGDN), this method is using nuclear magnetic resonance spectroscopy internal standard method to water
Divide content to carry out accurate quantitative analysis, has many advantages, such as that easy to operate, sampling quantity is few, reproducible.Technical solution is specific as follows:
(1) it accurately weighs 5~15mg of internal standard compound (being accurate to 0.1mg), 0.5~0.8ml of deuterated solvent dissolution, transfer is added
Into nuclear magnetic tube, membrana oralis sealing is sealed up.Prepared sample solution is placed in 10~20s of concussion in ultrasonic oscillation instrument, later
Nuclear magnetic resonance spectroscopy test is carried out to sample.The quantitative nuclear-magnetism test condition are as follows: nmr spectrometer resonant frequency be 400~
800MHz, 20-35 DEG C of temperature, delay time is 30s~60s, 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 diethylent glycol dinitrate is added, then seal up membrana oralis
Sealing, and shaken with ultrasonic oscillation instrument to uniformly mixed.Core is carried out again to the sample after addition diethylent glycol dinitrate
The spectrum test of magnetic resonance hydrogen, 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-diethylent glycol dinitrate 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 diethylent glycol dinitrate sample water characteristic signal peak peak area；
A2The peak area at the water characteristic signal peak of the sample of-addition diethylent glycol dinitrate；
Preferably, moisture content detection method in above-mentioned test diethylent glycol dinitrate sample, in the step (1) in
Mark object is hexamethyldisiloxane, benzene, paracide high sterling or standard substance, and deuterated solvent is deuterated dimethyl sulfoxide
(DMSO).Benzene, paracide and hexamethyldisiloxane not with diethylent glycol dinitrate component reaction, favorable solubility, and
It is easier to obtain high sterling or purity rubric substance, all hydrogen is in identical chemical environment, i.e. hydrogen nuclear magnetic resonance in substance
It composes and all there was only one group of characteristic peak in spectrogram, the internal standard compound requirement of nucleus magnetic hydrogen spectrum is quantified suitable for this system.The selection of deuterated solvent
Mainly according to the solvent borne of internal standard compound and sample, deuterated acetone or deuterium is can be selected in the solvent borne of comprehensive diethylent glycol dinitrate
Be solvent for dimethyl sulfoxide, but in an experiment discovery sample size is close and water content it is similar under the conditions of, deuterated DMSO solvent
Water peak is that peak shape is sharp and symmetrical single absorption peak in sample, and water characteristic peak is asymmetric double in deuterated acetone solvent samples
Peak, analysis are since hydrogen atom can generate fast exchange in D-atom in deuterated acetone and water, i.e., a hydrogen atom is by D-atom
Substituted hydrone content increases, and eventually leads to water peak in nuclear magnetic spectrogram and has occurred and splits point.Carrying out nuclear-magnetism characteristic peak integrating meter
It is symmetrically unimodal to generate smaller integral calculation error in contrast when calculation.Consider that the effumability of acetone may simultaneously
Sample nuclear magnetic spectrogram stability is had an impact, comprehensive analysis consideration selects deuterated dimethyl sulfoxide as diethylene glycol dinitric acid
Ester system quantifies the dicyandiamide solution of nuclear-magnetism detection
Preferably, diethylent glycol dinitrate sample weighting amount should be 2-3 times of internal standard compound in experiment.The control of this condition 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 do not answer phase
Poor multiple is excessive, and discovery control is in 1:10 between 10:1 in specific practical operation, and quantitative integration is to brought by final result
Error is smaller.Therefore comprehensively consider the factors such as moisture content in diethylent glycol dinitrate sample, internal standard compound molecular weight, determine two
Dinitroglycol 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 it
Than controlling in the above range, basis is detected 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 diethylent glycol dinitrate sample.Integral difference assay is taken with regard to the design of this problem
The accurate calculating of moisture content in sample is carried out, i.e., is only added in deuterated solvent to not adding diethylent glycol dinitrate first
Internal standard compound sample carries out quantitative nuclear-magnetism detection, obtains integrated area value of the water peak relative to internal standard compound characteristic peak in this system,
It is precisely weighed into nuclear-magnetism sample again and diethylent glycol dinitrate sample is added, quantitative core is then carried out with same experiment condition
Magnetic testi further obtains integrated area value of the water peak relative to internal standard compound in this system.The mechanism tested by quantitative nuclear-magnetism,
Although the integral area of characteristic peak simultaneously not absolute terms in nuclear magnetic spectrogram, does not have comparativity theoretically in not cospectral graph, by
The internal standard compound magnitude contained in test twice is constant, and test condition is identical, therefore the condition in stable condition in instrument test
Lower internal standard peak peak height, peak shape and peak position remain unchanged, value added of the water peak relative to the integrated area value of internal standard compound characteristic peak,
It is directly proportional with moisture magnitude contained in diethylent glycol dinitrate, it can be calculated by quantitative nuclear-magnetism formula.Simultaneously because
The resonant frequency of nuclear magnetic resonance spectrometer is higher, i.e., power is higher, and correspondingly resolution ratio, sensitivity and sampling stability all can be significant
It improves.Therefore for the analysis calibrating of micro-moisture in diethylent glycol dinitrate system, the nuclear-magnetism of global alignment different capacity
The Stability and veracity of spectrometer testing result, optimal selection 800M nmr spectrometer carry out quantitative detection, can get signal-to-noise ratio more
Good 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 diethylent glycol dinitrate system,
Test of many times finally considers the fast and easy of the accuracy of experimental result, reproducibility and detection method simultaneously, final to determine
The delay time of 30s-60s is selected, this parameter area can guarantee that internal standard compound and water all reach complete relaxation and restores balance
State, to guarantee on the basis of internal standard compound content to the accuracy of water and basis weight.
Diethylent glycol dinitrate sample weighting amount is 10-30mg in the present invention, although this is because improving dosing accuracy, drop
The demand of low error will configure highly concentrated solution as far as possible to reach the better signal-to-noise ratio of spectrogram, but sample solution concentration mistake simultaneously
Height may cause that solute Distribution in solution is uneven, and viscosity is excessive, cause spectral line broadening, while subtracting as far as possible for safety issue
Few diethylent glycol dinitrate dosage.Therefore sample weighting amount is limited in 10-30mg, has not only reached preferable signal-to-noise ratio but also has kept solution
Uniformity and free-running property.
Compared to the prior art, the master of above-mentioned diethylent glycol dinitrate moisture content detection method established by the present invention
It is few to have the beneficial effect that sample size dosage is taken in (1) test, effectively prevents conventional aqueous detection method due to the sample amount of taking
Security risk caused by big；(2) test method solves high sense as non-destructive testing without external forces such as friction, electrostatic substantially
Degree nitrate is under outside energy effect the problem of sensitive explosive；(3) test is simple, convenient and rapid, can be completed with rapid batch, real
Precision height, favorable reproducibility are tested, there is higher sensitivity, and without standard reference material or draw working curve；(4) method combines
Internal standard method and integral difference assay, having effectively removed other than sample residual moisture in reagent influences test bring.In summary,
The method of the moisture content of quantitative nuclear magnetic resonance spectroscopy, is suitable for this kind of high-energy of diethylent glycol dinitrate, high sensitivity and height
The analysis detection of risk sample provides a fast quantification for the trace moisture analysis detection of same type explosive wastewater product
Method and thinking.
Detailed description of the invention
Fig. 1 is the nucleus magnetic hydrogen spectrum spectrogram of diethylent glycol dinitrate
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
Diethylent glycol dinitrate1The foundation of H NMR spectra
1.1 instruments and sample
800 type NMR spectrometer with superconducting magnet of Bruker Ascend (German BRUKER company)；Mettler Toledo
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.)；Hexamethyldisiloxane high sterling (pacifies resistance to Jilin Chemical, purity
99%)；Diethylent glycol dinitrate (Xi'an Inst. of Modern Chemistry).
The preparation and measurement of 1.2 samples to be tested
Internal standard compound hexamethyldisiloxane 5-15mg is accurately weighed in 5mm nuclear magnetic tube, the deuterated dimethyl of 0.5ml is then added
Sulfoxide is sealed with sealed membrane after mixing, and prepared nuclear-magnetism sample is directly used in1H NMR test.After test,
It is removed again to the nuclear-magnetism sample cell for completing test, after addition diethylent glycol dinitrate 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, measuring temperature 300K, 30 ° 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, comprehensive diethylent glycol dinitrate chemical property are right using Topspin 3.5
Detection gained1H NMR spectra calibrated, baseline correction and phase adjustment, divides situation according to the coupling at proton signal peak column
And chemical displacement value is belonged to accordingly, as shown in table 1 below.The water proton signals peak and chemical potential of chemical shift δ 3.32
The hexamethyldisiloxane signal peak for moving δ 0.02 separates well and symmetrically and evenly with other signal peaks, meets the basic of quantitative nuclear-magnetism
Condition.
2 diethylent glycol dinitrate nucleus magnetic hydrogen spectrum Spectra peak recognition table of table
1.4 methodological study
Stability: taking with a diethylent glycol dinitrate 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, calculates
RSD value；
Repeatability: taking 6 parts of same batch diethylent glycol dinitrate, 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 a diethylent glycol dinitrate 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 diethylent glycol dinitrate sample, carries out according to above-mentioned experiment condition and method1After 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 is real
It tests, records the relative integral area of water peak to calculate moisture relative amount, calculate the rate of recovery.
Linear verification: taking same batch diethylent glycol dinitrate sample, and precision weighs sample about 10mg, 15mg, 20mg,
25mg is carried out according to above-mentioned experiment condition and method respectively1H NMR experiment records 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 diethylent glycol dinitrate moisture methodological study result of table
Embodiment 2
Moisture content in nuclear magnetic resonance hydrogen spectruming determining different batches diethylent glycol dinitrate
Internal standard compound hexamethyldisiloxane 5.3mg is accurately weighed in 5mm nuclear magnetic tube, the deuterated dimethyl of 0.6ml is then added
Sulfoxide is sealed with sealed membrane after mixing, and prepared nuclear-magnetism sample is directly used in1H NMR test, test parameter and item
Part are as follows: observing frequency 800.3MHz, measuring temperature 300K, 90 ° of pulses, 3 μ s of spectrum width, sampled data points 65536, scanning times 64
It is secondary, delay time 40s.The nuclear-magnetism sample cell that test is completed is removed again, diethylent glycol dinitrate 12mg is added and is sufficiently mixed
Afterwards, membrana oralis sealing is sealed up, then by sample with the progress of same test condition1H NMR test.By the same way to three batches of differences batch
Number diethylent glycol dinitrate sample detected, record nmr spectrum, calculate moisture content, as a result such as the following table 3.
3 different batches diethylent glycol dinitrate determination of moisture of table
| Lot number | Water content/% |
| 180321 | 0.857 |
| 180414 | 0.969 |
| 180505 | 0.547 |
You need to add is that above-mentioned specific embodiment is retouched to what the moisture detecting method of diethylent glycol dinitrate carried out
It is illustrative and non-limiting for stating, and above embodiments 1-2 is not the implementable whole embodiments of this patent, can be according to limited range
More examples, therefore the modifications and variations in the case where not departing from present general inventive concept are specifically enumerated again, belong to the scope of the present invention
Within.
The present invention establishes the nuclear magnetic resonance spectroscopy trace water content of diethylent glycol dinitrate, solves tradition
The big safety problem of detection method amount of samples is prominent, needs one-to-one standard substance, the problems such as method is cumbersome, test
It is few to take sample size dosage, test method is lossless and substantially without external forces such as friction, electrostatic, effectively prevents conventional aqueous inspection
Survey method is since macro-analysis dosage is big and high sensitivity nitrate the problem of sensitive explosive, is tested under outside energy effect
It is simple, convenient and rapid, it can be completed with rapid batch, experiment precision is high, favorable reproducibility has in combination with internal standard method and integral difference assay
Effect, which eliminates other than sample residual moisture in reagent, influences test bring.Especially suitable for high-energy, high sensitivity, high-risk
Property diethylent glycol dinitrate sample detection, for the quality of explosive wastewater raw material and product control provide effective analysis method
And means.
Claims (4)
1. a kind of method of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate (DEGDN) moisture content, it is characterised in that packet
Containing 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
Envelope.Prepared sample solution is placed in 10~20s of concussion in ultrasonic oscillation instrument, nuclear magnetic resonance spectroscopy is carried out to sample later
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 30s~60s, 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 diethylent glycol dinitrate is added, then to seal up membrana oralis close
Envelope, and shaken with ultrasonic oscillation instrument, nuclear magnetic resonance spectroscopy survey is carried out again to the sample after addition diethylent glycol dinitrate
Examination, the quantitative nuclear-magnetism test condition are 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 diethylent glycol dinitrate samplesFor the relative molecular mass of internal standard compound, MxFor the relative molecular mass of water,
HsFor the number of resonant nucleus in the functional group of 1 mole of internal standard compound characteristic signal, HxIt is generated in the functional group of signal altogether for 1 mole of water
The number of vibration core, AsFor the peak area at internal standard compound characteristic signal peak, A1It is special for water that the sample of diethylent glycol dinitrate is not added
Levy the peak area of signal peak, A2For the peak area at the water characteristic signal peak of the sample of addition diethylent glycol dinitrate.
2. the method for nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content according to claim 1, which is characterized in that
Deuterated solvent used is attached most importance to hydrogen dimethylamino base sulfoxide.
3. the method for nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content according to claim 1, internal standard compound used
It is required that for high sterling or hexamethyldisiloxane, benzene or the paracide of standard items.
4. according to the method for claim 3 nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content, which is characterized in that
Diethylent glycol dinitrate sample-adding quality should be 2-3 times of internal standard compound.
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