CN109239121A - A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate moisture content - Google Patents
A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate moisture content Download PDFInfo
- Publication number
- CN109239121A CN109239121A CN201811249906.1A CN201811249906A CN109239121A CN 109239121 A CN109239121 A CN 109239121A CN 201811249906 A CN201811249906 A CN 201811249906A CN 109239121 A CN109239121 A CN 109239121A
- Authority
- CN
- China
- Prior art keywords
- triethylene glycol
- glycol dinitrate
- sample
- nuclear magnetic
- internal standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- High Energy & Nuclear Physics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Toxicology (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of a kind of methods for measuring nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate (TEGDN) 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 triethylene 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 in triethylene glycol dinitrate (TEGDN) 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 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.Triethylene glycol dinitrate (TEGDN) is popular as Recent study
Energetic plasticiser, it is excellent since its is cheap, glass transition temperature is low, cryogenic mechanics performance is good and basic components burn rate is low etc.
Benign energy, has a good application prospect as the energetic plasticiser in high-energy propellant of new generation.
Due to atmosphere moisture diffusion and raw material are not dry etc., in the triethylene glycol dinitrate that produces
Contain a certain amount of moisture in usually, and the moisture content in triethylene glycol dinitrate is important to its stability, compatibility etc.
Physicochemical characteristic has extreme influence.Some researches show that contain under same period of storage by the high performance bond of matrix of nitrate
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, is realized in triethylene glycol dinitrate
The accurate detection of moisture content.Common trace water content has oven drying method, condensed steam water, Karl_Fischer method, near-infrared
Spectroscopic methodology etc., but due to triethylene glycol dinitrate high-energy, high sensitivity, high risk characteristic, for moisture detecting method
Have specific demand: (1) amount of samples should be lacked as far as possible, traditional for this point to reduce security risk in detection process
Oven drying method and drier, although being once applied to the detection of nitrate esters product moisture as standard method, as constant point
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 for test process
Security risk；(2) external forces such as friction, electrostatic should be avoided in test process as far as possible, to avoid high sensitivity nitrate in the external world
The lower explosion of energy effect.Iodine is ionized into iodine due to needing to generate electric current in test process by common karl Fischer moisture measurement method
Ion, and reaction process is monitored by electricity, the generation of inevitable electric current and charge during the test, it is clear that deposit
Using limitation；(3) test method should be simple, convenient and rapid as far as possible, and has higher sensitivity.Near infrared spectroscopy is used as opposite survey
Amount method, measurement sensitivity is higher, but its calibration needs one-to-one standard substance, and draws corresponding working curve, accordingly
Quantitative analysis work also higher cost, method it is cumbersome, for simple, convenient and rapid testing requirement, there is also limitations.(4) it tested
Cheng Zhongying avoids or excludes as far as possible influence of the moisture to measurement result in other additives and reagent and environmental condition.It is quantitative
Nuclear magnetic resonance (Quantitative nuclear magnetic resonance, qNMR) technology does not need determinand reference substance,
Sample pre-treatments step is easy, quick, can significantly improve detection efficiency, in recent years by United States Pharmacopeia, British Pharmacopoeia, European medicine
Allusion quotation, Chinese Pharmacopoeia (2010 editions) are included in succession.In recent years, due to nuclear magnetic resonance spectroscopy quantitative technique high sensitivity, qNMR technology
Using more and more extensive, obtained in terms of bulk pharmaceutical chemicals, pharmaceutical preparation, residual solvent measurement, sample component
It is widely applied.
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 triethylene glycol dinitrate moisture content, this method carry out moisture content using nuclear magnetic resonance spectroscopy internal standard method
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 internal standard compound 10-20mg (being accurate to 0.1mg), deuterated solvent 0.5-0.6ml dissolution, transfer is added
Into nuclear magnetic tube, membrana oralis sealing is sealed up.Prepared sample solution is placed in ultrasonic oscillation instrument and shakes 10-20s, it is right later
Sample carries 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, triethylene glycol dinitrate 20-40mg 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 triethylene 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-triethylene 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 triethylene glycol dinitrate sample water characteristic signal peak peak area；
A2The peak area at the water characteristic signal peak of the sample of-addition triethylene glycol dinitrate；
Preferably, moisture content detection method in above-mentioned test triethylene glycol dinitrate sample, in the step (1) in
Mark object is benzene, paracide, hexamethyldisiloxane high sterling or standard substance, and deuterated solvent is deuterated dimethyl sulfoxide
(DMSO).Benzene and paracide, hexamethyldisiloxane not with triethylene 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, the solvent borne of comprehensive triethylene glycol dinitrate and internal standard compound be can be selected deuterated
Acetone or deuterated dimethyl sulfoxide are solvent, but discovery sample size is close in an experiment and water content it is similar under the conditions of, it is deuterated
Water peak is that peak shape is sharp and symmetrical single absorption peak in DMSO solvent samples, and water characteristic peak is not right in deuterated acetone solvent samples
What is claimed is bimodal, and analysis is since hydrogen atom can generate fast exchange, i.e. a hydrogen atom quilt in D-atom in deuterated acetone and water
The hydrone content that D-atom replaces increases, and eventually leads to water peak in nuclear magnetic spectrogram and has occurred and splits point.Carrying out nuclear-magnetism characteristic peak
It is symmetrically unimodal to generate smaller integral calculation error in contrast when integral calculation.The effumability of acetone is considered simultaneously
Sample nuclear magnetic spectrogram stability may be had an impact, comprehensive analysis consideration selects deuterated dimethyl sulfoxide as triethylene glycol
Dinitrate system quantifies the dicyandiamide solution of nuclear-magnetism detection
Preferably, triethylene 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, internal standard compound molecular weight in triethylene glycol dinitrate sample, determine three
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 triethylene 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 triethylene glycol dinitrate is not added first
Add internal standard compound sample to carry out quantitative nuclear-magnetism detection, obtains integral area of the water peak relative to internal standard compound characteristic peak in this system
Value, then precisely weighed into nuclear-magnetism sample and triethylene glycol dinitrate sample is added, then determined with same experiment condition
Nuclear-magnetism detection is measured, integrated area value of the water peak relative to internal standard compound in this system is further obtained.It is tested by quantitative nuclear-magnetism
Mechanism, although the integral area of characteristic peak simultaneously not absolute terms in nuclear magnetic spectrogram, 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 in stable condition in instrument test
Under the conditions of internal standard peak peak height, peak shape and peak position remain unchanged, increasing of the water peak relative to the integrated area value of internal standard compound characteristic peak
It is value added directly proportional with moisture magnitude contained in triethylene glycol dinitrate, it can be calculated by quantitative nuclear-magnetism formula.Simultaneously
Since 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
It significantly improves.Therefore for the analysis calibrating of micro-moisture in triethylene glycol dinitrate, 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 triethylene 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 20s-50s 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.
Triethylene glycol dinitrate sample weighting amount is 20-40mg 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 triethylene glycol dinitrate dosage.Therefore sample weighting amount is limited in 20-40mg, 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 triethylene glycol dinitrate moisture content detection method established by the present invention
Have the beneficial effect that (1) test take sample size in milligram rank, dosage is few, effectively prevent conventional aqueous detection method by
In macro-analysis dosage security risk caused greatly；(2) test method is lossless and substantially without the external forces such as friction, electrostatic, solution
High sensitivity nitrate determined under outside energy effect the problem of sensitive explosive；(3) test is simple, convenient and rapid, can be with rapid batch
It completes, experiment precision height, favorable reproducibility, there is higher sensitivity, and without standard reference material or draw working curve；(4)
Method combination internal standard method and integral difference assay, having effectively removed other than sample residual moisture in reagent influences test bring.
In summary, the method for the moisture content of quantitative nuclear magnetic resonance spectroscopy, is suitable for this kind of high-energy of triethylene glycol dinitrate, height
The analysis detection of sensitivity and high risk sample provides one fastly for the trace moisture analysis detection of same type explosive wastewater product
Speed quantitative method and thinking.
Detailed description of the invention
Fig. 1 is the nucleus magnetic hydrogen spectrum spectrogram of triethylene 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
Triethylene glycol dinitrate1The foundation and ownership 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%)；Triethylene glycol dinitrate (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 0.6ml 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 triethylene glycol dinitrate 30mg is sufficiently mixed, seals up membrana oralis sealing,
Again by sample with the progress of same test condition1H NMR is tested, wherein test parameter and condition are as follows: observing frequency 800.3MHz is surveyed
Determine 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 triethylene glycol dinitrate, using Topspin 3.5
To detection gained1H NMR spectra calibrated, baseline correction and phase adjustment, divides feelings according to the coupling at proton signal peak column
Condition and chemical displacement value are belonged to accordingly, as shown in table 1 below.The water proton signals peak of chemical shift δ 3.33, and chemistry
It is displaced the benzene proton signal peak of δ 7.37, is separated with other signal peaks well and symmetrically and evenly, meets the basic item of quantitative nuclear-magnetism
Part.
1 triethylene glycol dinitrate nucleus magnetic hydrogen spectrum Spectra peak recognition table of table
1.4 methodological study
Stability: taking with a triethylene 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, meter
Calculate RSD value；
Repeatability: taking same 6 parts of batch triethylene 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 triethylene 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 triethylene 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
Experiment records the relative integral area of water peak to calculate moisture relative amount, calculates the rate of recovery.
Linear verification: taking same batch triethylene glycol dinitrate sample, and precision weighs sample about 20mg, 25mg, 30mg,
40mg 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 triethylene glycol dinitrate moisture methodological study result of table
Embodiment 2
Moisture content in nuclear magnetic resonance hydrogen spectruming determining different batches triethylene glycol dinitrate
Internal standard compound hexamethyldisiloxane 12mg 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, triethylene glycol dinitrate 25mg 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 triethylene glycol dinitrate sample detected, record nmr spectrum, calculate moisture content, as a result such as the following table 3.
3 different batches triethylene glycol dinitrate determination of moisture of table
| Lot number | Water content/% |
| 180321 | 0.862 |
| 180508 | 0.632 |
| 180521 | 0.836 |
You need to add is that above-mentioned specific embodiment is retouched to what the moisture detecting method of triethylene 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 triethylene 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 triethylene 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 triethylene glycol dinitrate (TEGDN) moisture content, it is characterised in that packet
Containing step in detail below:
(1) 10~20mg of internal standard compound is weighed, 0.5~0.8ml of deuterated reagent dissolution is added, is transferred in nuclear magnetic tube, seals up membrana oralis
Prepared sample solution is placed in 10~20s of concussion in ultrasonic oscillation instrument, carries out hydrogen nuclear magnetic resonance to sample later by sealing
Spectrum test.The quantitative nuclear-magnetism test condition are as follows: nmr spectrometer resonant frequency is 400~800MHz, 20~35 DEG C of temperature, is prolonged
The slow 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, 20~40mg of triethylene 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 triethylene 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 triethylene 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 triethylene 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 triethylene glycol dinitrate.
2. the method for nuclear magnetic resonance hydrogen spectruming determining triethylene 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 triethylene glycol dinitrate moisture content according to claim 1, internal standard compound used
It is required that for high sterling or benzene, paracide or the hexamethyldisiloxane of standard items.
4. according to the method for claim 3 nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate moisture content, which is characterized in that
Triethylene glycol dinitrate sample-adding quality should be 2-3 times of internal standard compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811249906.1A CN109239121B (en) | 2018-10-25 | 2018-10-25 | Method for measuring water content of triethylene glycol dinitrate by nuclear magnetic resonance hydrogen spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811249906.1A CN109239121B (en) | 2018-10-25 | 2018-10-25 | Method for measuring water content of triethylene glycol dinitrate by nuclear magnetic resonance hydrogen spectrum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109239121A true CN109239121A (en) | 2019-01-18 |
| CN109239121B CN109239121B (en) | 2021-07-27 |
Family
ID=65082030
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811249906.1A Active CN109239121B (en) | 2018-10-25 | 2018-10-25 | Method for measuring water content of triethylene glycol dinitrate by nuclear magnetic resonance hydrogen spectrum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109239121B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1718072A1 (en) * | 1990-03-29 | 1992-03-07 | Особое Конструкторско-Технологическое Бюро С Экспериментальным Производством Института Химии Поверхности Ан Усср | Method of determination of water content |
| CN105021643A (en) * | 2014-04-18 | 2015-11-04 | 中国石油化工股份有限公司 | Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument |
| WO2016179632A1 (en) * | 2015-05-08 | 2016-11-17 | Sipco Pty Ltd | An apparatus and method for the near real time physical analysis of hay or cotton bales using nuclear magnetic resonance techniques |
-
2018
- 2018-10-25 CN CN201811249906.1A patent/CN109239121B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1718072A1 (en) * | 1990-03-29 | 1992-03-07 | Особое Конструкторско-Технологическое Бюро С Экспериментальным Производством Института Химии Поверхности Ан Усср | Method of determination of water content |
| CN105021643A (en) * | 2014-04-18 | 2015-11-04 | 中国石油化工股份有限公司 | Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument |
| WO2016179632A1 (en) * | 2015-05-08 | 2016-11-17 | Sipco Pty Ltd | An apparatus and method for the near real time physical analysis of hay or cotton bales using nuclear magnetic resonance techniques |
Non-Patent Citations (2)
| Title |
|---|
| 国家药典委员会 编著: "《中国药典分析检测技术指南》", 31 July 2017 * |
| 赵羽 等: "重水氘代率的NMR测定方法", 《现代仪器》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109239121B (en) | 2021-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109030538A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining nitroglycerine moisture content | |
| CN111007098A (en) | Quantitative nuclear magnetic hydrogen spectrum value determination method for 2,4, 6-trinitrotoluene standard substance | |
| CN108827998B (en) | Method for accurately measuring purity of volatile substance by adopting quantitative nuclear magnetic resonance hydrogen spectrum | |
| CN112305007B (en) | Method for measuring deuterium isotope abundance of deuterium labeled compound by using nuclear magnetic hydrogen spectrum or deuterium spectrum | |
| CN109239120A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining 1,2- Propylene Glycol Dinitrate moisture content | |
| CN109030539B (en) | Method for measuring moisture content of 1, 5-diazido-3-nitro-3-aza pentane by nuclear magnetic resonance hydrogen spectrum | |
| CN111971570B (en) | Method for quantitative determination of heteronuclear by nuclear magnetic resonance spectroscopy, reference substance thereof and method for determination of deuteration degree of deuterated compound | |
| CN106018456A (en) | Method for determining purity of daptomycin on basis of hydrogen nuclear magnetic resonance | |
| CN109030535A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate moisture content | |
| CN109030536A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate and nitroglycerine naked nitric acid ester moisture content | |
| CN109030537A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining butanetriol trinitrate and nitroglycerine naked nitric acid ester moisture content | |
| CN109030540A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining diethylent glycol dinitrate and nitroglycerine naked nitric acid ester moisture content | |
| CN109239121A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining triethylene glycol dinitrate moisture content | |
| Gong et al. | Purity assessment of luteolin reference material candidates by coulometric titration method | |
| CN115166080B (en) | Method for detecting impurity A and impurity B in ifosfamide bulk drug | |
| CN116626087A (en) | Method for quantitatively analyzing allyl sucrose ether content through nuclear magnetic resonance hydrogen spectrum | |
| CN106124550A (en) | A kind of method quickly measuring vildagliptin purity based on hydrogen nuclear magnetic resonance | |
| CN105954310A (en) | Method for rapidly measuring purity of bulk pharmaceutical chemical of lincomycin hydrochloride on basis of hydrogen-nuclear magnetic resonance | |
| CN111007097A (en) | Quantitative nuclear magnetic hydrogen spectrum valuing method for 2, 6-dinitrotoluene standard substance | |
| CN108398452A (en) | A method of ginsenoside Re's reference substance content is measured based on proton magnetic quantitative analysis tech | |
| CN114018965A (en) | Quantitative detection technology of polysaccharide by nuclear magnetic resonance hydrogen spectrometry | |
| CN115128177A (en) | Method for analyzing and determining genotoxic impurities in ganciclovir condensation compound by using HPLC method | |
| CN111060548B (en) | Quantitative nuclear magnetic hydrogen spectrum value-fixing method for pentaerythritol standard substance | |
| CN108593696B (en) | Method for determining trifluoroacetic acid residue in polypeptide by using quantitative nuclear magnetism | |
| Li et al. | 1 H NMR determination of 1, 3-dicyclohexylurea, glutaric acid and triethylamine in medical four-arm poly (ethylene glycol)-N-hydroxysuccinimide-glutarate for better quality control |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |