CN109030539A - A kind of method of nuclear magnetic resonance hydrogen spectruming determining 1,5- diazido -3- nitro -3- aza-pentane moisture content - Google Patents
A kind of method of nuclear magnetic resonance hydrogen spectruming determining 1,5- diazido -3- nitro -3- aza-pentane moisture content Download PDFInfo
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Abstract
The invention discloses a kind of nuclear magnetic resonance hydrogen spectruming determinings 1, the method of 5- diazido -3- nitro -3- aza-pentane (DIANP) 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 1,5- diazido -3- nitro -3- aza-pentane 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 1,5- diazido -3- nitro -3- aza-pentane 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 1, bis- nitrine of 5-
The method of base -3- nitro -3- aza-pentane (DIANP) moisture content belongs to explosive wastewater product analysis detection field.
Background technique
1,5- diazido -3- nitro -3- aza-pentane (DIANP) is used as Azido Energetic plasticizer, has high energy, Gao Ran
The features such as speed, low burn temperature, small big level-one combustion gas relative molecular weight of gas production, it is now widely used for propellant, pyrotechnic compound, gas
The fields such as propellant and high force-low flame temperature gun propellant.It is raw due to atmosphere moisture diffusion and raw material are not dry etc.
It produces in usual in obtained 1,5- diazido -3- nitro -3- aza-pentane containing a certain amount of moisture, content is stable
An important factor for important physicochemical characteristics such as property, compatibility.It is required in the operating specification of certain class composite explosives, moisture content is not
It obtains and is higher than 0.5%, therefore in actual production and storage process, need strict control wherein moisture content, realize to 1,5- bis-
The accurate detection of moisture content in azido -3- nitro -3- aza-pentane.Common trace water content have oven drying method,
Condensed steam water, Karl_Fischer method, near infrared spectroscopy etc., but since 1,5- diazido -3- nitro -3- aza-pentane is as folded
Nitrogen compound high-energy, high sensitivity, high risk characteristic, have specific demand for moisture detecting method: (1) sample takes
Dosage should be lacked as far as possible, to reduce security risk in detection process.Traditional oven drying method and drier, although being once used as standard method
Applied to the detection of explosive wastewater class product moisture, but as macro-analysis method (test is with sample amount generally in 5~10g), it is clear that
Since sample size is excessive, so that taking, there are biggish security risks for test process；(2) it should avoid rubbing as far as possible in test process
Under outside energy effect combustion explosion occurs for the external forces such as wiping, electrostatic, shock to avoid high sensitivity azido compound.Often
Iodine is ionized into iodide ion due to needing to generate electric current in test process by karl Fischer moisture measurement method, and passes through electricity pair
Reaction process is monitored, the generation of inevitable electric current and charge during the test, it is clear that is existed using limitation；(3) it surveys
Method for testing should be simple, convenient and rapid as far as possible, and has higher sensitivity.Near infrared spectroscopy as relative measurement method, measurement sensitivity compared with
Height, but its calibration needs one-to-one standard substance, and draws corresponding working curve, corresponding quantitative analysis work also at
This is higher, method is cumbersome, and for simple, convenient and rapid testing requirement, there is also limitations.(4) it should avoid or arrange as far as possible in test process
Except influence of the moisture to measurement result in other additives and reagent and environmental condition.Quantitative nuclear magnetic resonance
(Quantitative nuclearmagnetic resonance, qNMR) technology does not need determinand reference substance, before sample
It is easy, quick to manage step, detection efficiency can be significantly improved, in recent years by United States Pharmacopeia, British Pharmacopoeia, European Pharmacopoeia, China
Pharmacopeia (2010 editions) is included in succession.In recent years, due to nuclear magnetic resonance spectroscopy quantitative technique high sensitivity, the application of qNMR technology is got over
Come it is more extensive, bulk pharmaceutical chemicals, pharmaceutical preparation, residual solvent measurement, sample component in terms of obtained widely answering
With.
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 1,5- diazido -3- nitro -3- aza-pentane (DIANP), this method use nuclear magnetic resonance
Hydrogen composes internal standard method and carries out accurate quantitative analysis to moisture content, has many advantages, such as that easy to operate, sampling quantity is few, reproducible.Technical side
Case is specific as follows:
(1) 5~15mg of internal standard compound is accurately weighed, 0.5~0.8ml of deuterated solvent dissolution is added, is transferred in nuclear magnetic tube, adds
Sealed membrane sealing.Prepared sample solution is placed in ultrasonic oscillation instrument after concussion mixing, nuclear-magnetism is carried out to sample later
The hydrogen spectrum that resonates is tested.The quantitative nuclear-magnetism test condition are as follows: nmr spectrometer resonant frequency is 400~800MHz, temperature 20-35
DEG C, delay time 30s-60s, pulse angle is 30~90 °, and sampling number is 32-128 times.
(2) the nuclear-magnetism sample cell that test is completed is removed, addition 1,5- diazido -3- nitro -3- aza-pentane 20~
40mg, then membrana oralis sealing is sealed up, and shaken to uniformly mixed with ultrasonic oscillation instrument.To addition 1,5- diazido -3- nitro -
Sample after 3- aza-pentane carries out nuclear magnetic resonance spectroscopy test again, and the quantitative nuclear-magnetism test condition and previous step are kept
Unanimously.
(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 -1,5- diazido -3- nitro -3- aza-pentane 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 1,5- diazido -3- nitro -3- aza-pentane sample water characteristic signal peak peak area；
A2The peak area at the water characteristic signal peak of-addition 1,5- diazido -3- nitro -3- aza-pentane sample；
Preferably, above-mentioned test 1, moisture content detection method in 5- diazido -3- nitro -3- aza-pentane sample,
Internal standard compound is hexamethyldisiloxane, benzene and 1 in the step (1), 1,2,2 ,-tetrachloroethanes high sterling or standard substance are deuterated
Solvent is deuterated dimethyl sulfoxide (DMSO).Hexamethyldisiloxane, benzene and 1,1,2,2 ,-tetrachloroethanes not with bis- nitrine of 1,5-
Base -3- nitro -3- aza-pentane component reaction, favorable solubility, and be easier to obtain high sterling or purity rubric substance, substance
In all hydrogen be in identical chemical environment, i.e., all there was only one group of characteristic peak in nuclear magnetic resonance spectroscopy spectrogram, be suitable for ontology
It is the internal standard compound requirement of quantitative nucleus magnetic hydrogen spectrum.The selection of deuterated solvent mainly according to the solvent borne of internal standard compound and sample, integrates 1,
5- diazido -3- nitro -3- aza-pentane and internal standard compound solvent borne, 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 consideration selects deuterated dimethyl sulfoxide as 1,5- diazido -3- nitro -3- aza-pentane system
The dicyandiamide solution of quantitative nuclear-magnetism detection
Preferably, 1,5- diazido -3- nitro -3- aza-pentane sample weighting amount should be 1-3 times of internal standard compound in experiment.This
The control of one condition is since in the test of quantitative nuclear-magnetism, one important condition is that two characteristic peaks contrasted integrate face
It is excessive that the ratio between product value should not differ multiple, and discovery control is in 1:10 between 10:1 in specific practical operation, and quantitative integration is to most
The error brought by fruit that terminates is smaller.Therefore comprehensively consider moisture in 1,5- diazido -3- nitro -3- aza-pentane sample to contain
The factors such as amount, internal standard compound molecular weight determine that 1,5- diazido -3- nitro -3- aza-pentane sample weighting amount should be the 1-3 of internal standard compound
This condition again may make internal standard compound characteristic peak and water peak area ratio to control in the above range, as suitable quantitative core
Magnetic testi basis.
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, Accurate Determining 1, the content of micro-moisture in 5- diazido -3- nitro -3- aza-pentane sample.This problem is designed
Integral difference assay is taken to carry out the accurate calculating of moisture content in sample, i.e., first to not adding 1,5- diazido -3- nitro -
3- aza-pentane only adds internal standard compound sample in deuterated solvent and carries out quantitative nuclear-magnetism detection, and it is opposite to obtain water peak in this system
In the integrated area value of internal standard compound characteristic peak, then is precisely weighed into nuclear-magnetism sample and 1,5- diazido -3- nitro -3- nitrogen is added
Then miscellaneous pentane sample carries out quantitative nuclear-magnetism detection with same experiment condition, it is opposite further to obtain water peak in this system
In the integrated area value of internal standard compound.The mechanism tested by quantitative nuclear-magnetism, although the integral area of characteristic peak is not in nuclear magnetic spectrogram
Absolute value does not have comparativity theoretically in not cospectral graph, but the internal standard compound magnitude as contained in testing twice is constant, and
Test condition is identical, therefore internal standard peak peak height, peak shape and peak position remain unchanged under conditions of instrument test is in stable condition, water
Peak is relative to the value added of the integrated area value of internal standard compound characteristic peak and 1, institute in 5- diazido -3- nitro -3- aza-pentane
The moisture magnitude contained is directly proportional, can be calculated by quantitative nuclear-magnetism formula.Simultaneously because the resonant frequency of nuclear magnetic resonance spectrometer
Higher, i.e., power is higher, and correspondingly resolution ratio, sensitivity and sampling stability can all significantly improve.Therefore folded for 1,5- bis-
The analysis calibrating of micro-moisture in nitrogen base -3- nitro -3- aza-pentane system, the nmr spectrometer detection of global alignment different capacity
As a result Stability and veracity, optimal selection 800M nmr spectrometer carry out quantitative detection, can get signal-to-noise ratio more preferably nuclear-magnetism
Hydrogen composes 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 1,5- diazido -3- nitro -3- aza-pentane system
Nuclear-magnetism behavioral study, test of many times finally considers the convenience of the accuracy of experimental result, reproducibility and detection method simultaneously
Rapidity, the final delay time for determining selection 30s-60s, 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.
1,5- diazido -3- nitro -3- aza-pentane sample weighting amount is 20-40mg in the present invention, although this is because mentioning
High 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 simultaneously
Sample solution excessive concentration may cause that solute Distribution in solution is uneven, and viscosity is excessive, cause spectral line broadening, while for peace
Full property problem reduces 1,5- diazido -3- nitro -3- aza-pentane dosage to the greatest extent.Therefore sample weighting amount is limited in 20-40mg,
Not only reach preferable signal-to-noise ratio but also keep the uniformity and free-running property of solution.
Compared to the prior art, above-mentioned 1,5- diazido -3- nitro -3- aza-pentane moisture established by the present invention contains
Quantity measuring method mainly to have the beneficial effect that sample size dosage is taken in (1) test few, effectively prevent conventional aqueous detection method
Due to the sample amount of taking security risk caused greatly；(2) test method is substantially without external forces such as friction, electrostatic, as lossless
Detection solves the problems, such as high sensitivity azido compound sensitive explosive under outside energy effect；(3) test is simple, convenient and rapid,
It can be completed with rapid batch, experiment precision height, favorable reproducibility have higher sensitivity, and be not necessarily to standard reference material or drafting
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 influences.In summary, the method for the moisture content of quantitative nuclear magnetic resonance spectroscopy, is suitable for 1,5- diazido -3- nitre
The analysis detection of the azido compound sample of this kind of high-energy of base -3- aza-pentane, high sensitivity and high risk is same type fire
The trace moisture analysis detection of explosive product provides the method and thinking of a fast quantification.
Detailed description of the invention
Fig. 1 is the nucleus magnetic hydrogen spectrum spectrogram of 1,5- diazido -3- nitro -3- aza-pentane
Fig. 2 is the chemical structural formula of 1,5- diazido -3- nitro -3- aza-pentane
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
1,5- diazido -3- nitro -3- aza-pentane1The foundation of HNMR map
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%)；1,5- diazido -3- nitro -3- aza-pentane (Xi'an Inst. of Modern Chemistry).
The preparation and measurement of 1.2 samples to be tested
Internal standard compound hexamethyldisiloxane 15mg is accurately weighed in 5mm nuclear magnetic tube, it is sub- that the deuterated dimethyl of 0.5ml is then added
Sulfone is sealed with sealed membrane after mixing, and prepared nuclear-magnetism sample is directly used in1HNMR test.After test, then to
The nuclear-magnetism sample cell that test is completed is removed, after addition 1,5- diazido -3- nitro -3- aza-pentane 20mg is sufficiently mixed,
Membrana oralis sealing is sealed up, then by sample with the progress of same test condition1H NMR is tested, wherein 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 64 times, delay time
40s。
1.3 sample1H H NMR spectroscopy map analysis
According to1H NMR spectra data in literature, comprehensive 1,5- diazido -3- nitro -3- aza-pentane chemical property, is adopted
Obtained by 3.5 pairs of detections of Topspin1H NMR spectra calibrated, baseline correction and phase adjustment, according to proton signal peak
Coupling column point situation and chemical displacement value belonged to accordingly, as shown in table 1 below.The water proton of chemical shift δ 3.32 is believed
The hexamethyldisiloxane signal peak at number peak and chemical shift δ 0.03 separates well and symmetrically and evenly, symbol with other signal peaks
Close the primary condition of quantitative nuclear-magnetism.
2 1,5- diazido -3- nitro -3- aza-pentane nucleus magnetic hydrogen spectrum Spectra peak recognition table of table
1.4 methodological study
Stability: taking with 1,5- of portion diazido -3- nitro -3- aza-pentane sample, according to above-mentioned experiment condition with
Method is carried out 0,2,4,6,8,12h respectively1H NMR experiment records the relative integral area of water peak to calculate the water of sample
Divide relative amount, calculates RSD value；
Repeatability: taking same batch 1,6 parts of aza-pentane of -3- nitro -3- of 5- diazido, according to above-mentioned experiment condition and
Method carries out1H NMR experiment records the relative integral area of water peak to calculate the moisture relative amount of sample, calculates RSD
Value；
Precision: taking with 1,5- of portion diazido -3- nitro -3- aza-pentane sample, according to above-mentioned experiment condition with
Method METHOD FOR CONTINUOUS DETERMINATION 6 times, the relative integral area of water peak is recorded to calculate the moisture relative amount of sample, calculates RSD value；
Recovery of standard addition: same batch 1,5- diazido -3- nitro -3- aza-pentane sample, according to above-mentioned experiment are taken
Condition and method carry out1It is then accurate that 2mg, 5mg pure water, after pure water is added every time, according to above is added after H NMR experiment
Method carries out1H 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 1,5- diazido -3- nitro -3- aza-pentane sample, and precision weighs sample about
20mg, 25mg, 30mg, 35mg are carried out according to above-mentioned experiment condition and method respectively1H NMR experiment records the relatively long-pending of water peak
Facet product 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 1,5- diazido -3- nitro -3- aza-pentane moisture methodological study result of table
Embodiment 2
Moisture content in nuclear magnetic resonance hydrogen spectruming determining different batches 1,5- diazido -3- nitro -3- aza-pentane
Internal standard compound hexamethyldisiloxane 10mg 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, test parameter and condition
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 128
It is secondary, delay time 40s.The nuclear-magnetism sample cell that test is completed is removed again, 1,5- diazido -3- nitro -3- azepine penta is added
After alkane 20mg is sufficiently mixed, membrana oralis sealing is sealed up, then by sample with the progress of same test condition1H NMR test.According to phase Tongfang
Method detects 1, the 5- diazido -3- nitro -3- aza-pentane sample of three batches of different lot numbers, records nuclear magnetic resoance spectrum
Figure calculates moisture content, as a result such as the following table 3.
3 different batches 1,5- diazido -3- nitro -3- aza-pentane determination of moisture of table
| Lot number | Water content/% |
| 180402 | 0.593 |
| 180509 | 0.536 |
| 171113 | 0.326 |
You need to add is that above-mentioned specific embodiment examines the moisture of 1,5- diazido -3- nitro -3- aza-pentane
Being described as survey method progress is illustrative and non-limiting, and above embodiments 1-2 is not the implementable whole embodiments of this patent, can
More examples, therefore the modifications and variations in the case where not departing from present general inventive concept are specifically enumerated again according to limited range, are belonged to
Within the scope of the present invention.
The present invention establishes the nuclear magnetic resonance spectroscopy micro-moisture detection of 1,5- diazido -3- nitro -3- aza-pentane
Method solves the prominent big safety problem of traditional detection method amount of samples, the one-to-one standard substance of needs, method operation
The problems such as cumbersome, test take that sample size dosage is few, and test method is lossless and substantially without external forces such as friction, electrostatic, effectively
Conventional aqueous detection method is avoided since macro-analysis dosage is big and high sensitivity azido compound is under outside energy effect
The problem of sensitive explosive, test is simple, convenient and rapid, can be completed with rapid batch, experiment precision height, 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.It is particularly suitable
In high-energy, high sensitivity, high risk 1,5- diazido -3- nitro -3- aza-pentane sample detection, be explosive wastewater raw material
And the quality control of product provides effective analysis method and means.
Claims (4)
1. a kind of nuclear magnetic resonance hydrogen spectruming determining 1, the method for 5- diazido -3- nitro -3- aza-pentane (DIANP), feature
It is comprising 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 ultrasonic oscillation instrument to nuclear magnetic resonance spectroscopy after shaking 30~60s to test, nuclear magnetic resonance
Hydrogen composes test condition are as follows: and nmr spectrometer resonant frequency is 400~800MHz, and 20~35 DEG C of temperature, delay time is 30s~60s,
Pulse angle is 30~90 °, and sampling number is 32~128 times；
(2) the nuclear-magnetism sample cell that test is completed is removed, 1,5- diazido -3- nitro -3- 20~40mg of aza-pentane is added,
Membrana oralis sealing is sealed up again, and is shaken with ultrasonic oscillation instrument, after 1,5- diazido -3- nitro -3- aza-pentane is added
Sample carries out nuclear magnetic resonance spectroscopy test again, and the quantitative nuclear-magnetism test condition 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 1,5- diazido -3- nitro -3- aza-pentane samplesFor the relative molecular mass of internal standard compound, MxFor water
Relative molecular mass, HsFor the number of resonant nucleus in the functional group of 1 mole of internal standard compound characteristic signal, HxSignal is generated for 1 mole of water
Functional group on resonant nucleus number, AsFor the peak area at internal standard compound characteristic signal peak, A1For 1,5- diazido -3- is not added
The peak area at the water characteristic signal peak of nitro -3- aza-pentane sample, A2For 1,5- diazido -3- nitro -3- azepine is added
The peak area at the water characteristic signal peak of pentane sample.
2. the side of nuclear magnetic resonance hydrogen spectruming determining 1,5- diazido -3- nitro -3- aza-pentane moisture content according to claim 1
Method, which is characterized in that deuterated solvent used is attached most importance to hydrogen dimethylamino base sulfoxide.
3. the side of nuclear magnetic resonance hydrogen spectruming determining 1,5- diazido -3- nitro -3- aza-pentane moisture content according to claim 1
Method, internal standard compound used require be high sterling or standard items benzene, 1,1,2,2 ,-tetrachloroethanes or hexamethyldisiloxane.
4. according to the side of claim 3 nuclear magnetic resonance hydrogen spectruming determining 1,5- diazido -3- nitro -3- aza-pentane moisture content
Method, which is characterized in that 1,5- diazido -3- nitro -3- aza-pentane sample-adding quality should be 1-3 times of internal standard compound.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111060548A (en) * | 2019-12-18 | 2020-04-24 | 西安近代化学研究所 | Quantitative nuclear magnetic hydrogen spectrum value-fixing method for pentaerythritol standard substance |
| CN113155935A (en) * | 2021-04-12 | 2021-07-23 | 山西钢科碳材料有限公司 | Method for measuring moisture content in azo initiator |
| CN115508400A (en) * | 2022-11-23 | 2022-12-23 | 中国石油大学(华东) | Method for determining content of benzyl quinoline quaternary ammonium salt dimer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111060548A (en) * | 2019-12-18 | 2020-04-24 | 西安近代化学研究所 | Quantitative nuclear magnetic hydrogen spectrum value-fixing method for pentaerythritol standard substance |
| CN111060548B (en) * | 2019-12-18 | 2023-03-17 | 西安近代化学研究所 | Quantitative nuclear magnetic hydrogen spectrum value-fixing method for pentaerythritol standard substance |
| CN113155935A (en) * | 2021-04-12 | 2021-07-23 | 山西钢科碳材料有限公司 | Method for measuring moisture content in azo initiator |
| CN115508400A (en) * | 2022-11-23 | 2022-12-23 | 中国石油大学(华东) | Method for determining content of benzyl quinoline quaternary ammonium salt dimer |
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