CN105866065A - Method of analyzing content of urotropine in urotropine-acetic acid solution - Google Patents
Method of analyzing content of urotropine in urotropine-acetic acid solution Download PDFInfo
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Substances CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 25
- 229960004011 methenamine Drugs 0.000 claims description 38
- 238000001228 spectrum Methods 0.000 claims description 23
- 239000011159 matrix material Substances 0.000 claims description 17
- 238000002235 transmission spectroscopy Methods 0.000 claims description 14
- 239000000470 constituent Substances 0.000 claims description 13
- 239000000052 vinegar Substances 0.000 claims description 11
- 235000021419 vinegar Nutrition 0.000 claims description 11
- 239000013598 vector Substances 0.000 claims description 9
- 238000012628 principal component regression Methods 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 8
- 238000011156 evaluation Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000002596 correlated effect Effects 0.000 claims description 3
- 230000000875 corresponding effect Effects 0.000 claims description 3
- 238000002790 cross-validation Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000013210 evaluation model Methods 0.000 claims description 3
- 238000000513 principal component analysis Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 108090000623 proteins and genes Proteins 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000002329 infrared spectrum Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000004445 quantitative analysis Methods 0.000 abstract description 6
- 238000009614 chemical analysis method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000002360 explosive Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- XQJMXPAEFMWDOZ-UHFFFAOYSA-N 3exo-benzoyloxy-tropane Natural products CN1C(C2)CCC1CC2OC(=O)C1=CC=CC=C1 XQJMXPAEFMWDOZ-UHFFFAOYSA-N 0.000 description 4
- QQXLDOJGLXJCSE-UHFFFAOYSA-N N-methylnortropinone Natural products C1C(=O)CC2CCC1N2C QQXLDOJGLXJCSE-UHFFFAOYSA-N 0.000 description 4
- QIZDQFOVGFDBKW-DHBOJHSNSA-N Pseudotropine Natural products OC1C[C@@H]2[N+](C)[C@H](C1)CC2 QIZDQFOVGFDBKW-DHBOJHSNSA-N 0.000 description 4
- CYHOMWAPJJPNMW-JIGDXULJSA-N tropine Chemical compound C1[C@@H](O)C[C@H]2CC[C@@H]1N2C CYHOMWAPJJPNMW-JIGDXULJSA-N 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000012886 linear function Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/127—Calibration; base line adjustment; drift compensation
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention relates to a method of analyzing content of urotropine in a urotropine-acetic acid solution, belongs to the field of explosive process and the technical field of near infrared spectrum quantitative analysis and aims to solve the problems of unstable production process and product yield and environment pollution caused by existing chemical analysis methods. The method includes: collecting and treating a sample in a certain concentration range; collecting near infrared spectra of the sample; using a chemical analysis method to measure concentration of the sample; building a mathematic relation between the near infrared spectra and a chemical analysis value; utilizing a quantitative analysis method to build a quantitative analysis model of urotropine. The method can replace the existing chemical analysis methods, and analysis results can be quickly acquired; no any solvent is used, so that environment protection is realized, and manpower cost and material cost can be lowered.
Description
Technical field
The present invention relates to hexamethylenamine content analysis method in a kind of hexamethylenamine-acetum, belong to Explosive Technology neck
Territory, Near-Infrared Spectra for Quantitative Analysis technical field.
Background technology
HMX (HMX) is current most widely used explosive, and the commonly used production method in present countries in the world is
Acetic anhydride method.In the production process of HMX, constituent content is quickly analyzed is key technology, and raw-material material is than not only affecting product matter
Amount and production cost, and production technology is had important impact.Hexamethylenamine is to produce former material important during HMX
Material, can increase the stability of raw material rate of charge, and then affect the yield of product and the matter of product the detection of hexamethylenamine
Amount.
At present, HMX produces hexamethylenamine detection containing quantitative analysis in preparation process and mainly uses chemical analysis method, due to
It is to be interrupted or off-line operation so that analytical cycle is long, it is impossible to enough production technologies of feeding back in time, and off-line sampling exists number
According to analyzing delayed problem, easily causing production technology unstable, product yield is unstable.Therefore, traditional conventional method is
Through the quick testing requirement of hexamethylenamine content cannot be met.So, hexamethylenamine-acetum in HMX production process to be realized
The quick analysis of middle hexamethylenamine content, needs to create a kind of quick, lossless detection method.
In recent years, Near-Infrared Spectra for Quantitative Analysis technology, because of its quick, lossless, environmental protection, is saved the advantages such as human cost and is existed
Every profession and trade achieves and is widely applied.Along with popularizing of this technology, this technology is gradually applied in explosive detection field.
But, the most domestic yet there are no relevant utilizes hexamethylenamine content in near-infrared spectrum technique detection hexamethylenamine-acetum
Report.
Summary of the invention
The invention aims to solve existing chemical analysis method cause production technology, product yield unstable and
The problem of environmental pollution, it is provided that hexamethylenamine content analysis method in a kind of hexamethylenamine-acetum.
It is an object of the invention to be achieved through the following technical solutions.
A kind of to hexamethylenamine content analysis method in hexamethylenamine-acetum, specifically comprise the following steps that
Step one, collect and process sample.Preparation sample be hexamethylenamine mass percentage content be 7%～11%
Hexamethylenamine-acetum, when carrying out the design of sample component concentration, should avoid linearly being correlated with between concentration of component.Sample
Number is no less than 60 parts, randomly chooses wherein more than 50 parts samples and participates in modeling as calibration set, and remaining sample is as checking collection.
Step 2, the NIR transmittance spectroscopy of mensuration calibration set sample.Tem analysis module is used to detect, with sky
Liquid-like QC is that background is scanned, and every part of sample parallel gathers 3 times～5 times, gathers spectral scan 32 times～64 times every time,
Take the averaged spectrum original spectrum modeling as this sample of sample parallel acquisition, spectral scan scope: 12000～4000cm-1,
Spectral resolution 8cm-1。
Step 3, set up model.The NIR transmittance spectroscopy of calibration set sample is carried out pretreatment, then with corresponding crow
Lip river tropine content is associated；Again by the bearing calibration of principal component regression method (PCR), set up NIR transmittance spectroscopy and crow Lip river
Calibration model between tropine content.Evaluation index according to model: coefficient R2, cross validation mean square deviation (RMSECV) and
Mean square deviation (RMSEC) is comprehensively analyzed, and determines optimal models.
Preprocess method described in step 3 uses single order or second-order differential, the filtering of Norris derivative, Savitzky-
One or more methods during Golay is smooth, can eliminate instrumental background or the drift impact on signal.
In step 3, the basic thought of principal component regression is exactly the main constituent first obtaining spectrum, resettles sample size and master
The linear correlation of composition, predicts the concentration of unknown sample with the linear function set up.
Calibration set light spectrum matrix X (n × k) of crow vinegar solution is decomposed into the apposition sum of k vector, is transformed to one newly
Main constituent matrix T, it may be assumed that
X=t1p1 T+t2p2 T+t3p3 T+…tkpk T
T=Xp/pTp
K=10 in optimal models, T=(t1, t2..., t10)
The least square solution of B: B=(TTT)-1TTC
C=TB+E
In formula, T is the orthogonal matrix that X principal component analysis obtains, and C is hexamethylenamine mass percentage content index, and B is for being
Matrix number, E is residual matrix, and n is calibration set sample number, and t is score vector, and p is load vectors (also referred to as main constituent or main cause
Son).In optimal models, calibration set sample number is 50, and optimal main cause subnumber k is 10.
Step 4, employing checking collection sample are predicted and evaluate optimal models.The near-infrared transmission light of each checking collection sample
Spectrum test at least 3 times, averages and carries out hexamethylenamine content analysis, analytical error, evaluation model.
Step 5, the quick of hexamethylenamine content of unknown sample measure.Collect new hexamethylenamine-acetum conduct
Unknown sample, gathers the NIR transmittance spectroscopy of all unknown sample, the model set up by step 3, it is possible to directly obtain crow
The content value of Lip river tropine.
The expansion of detection limit.According to the actual requirements, on the basis of existing model, by adding the sample of other concentration range
Transmitted spectrum, the detection limit of extendible method.
Beneficial effect
1, the inventive method existing chemistry point alternative to hexamethylenamine content analysis in hexamethylenamine-acetum is used
Analysis method, it is possible to quickly obtain analysis result, it is possible to decrease human cost, material cost.
2, existing analysis method uses titration assay method, and 3 testers spend analysis that 2 hours can be complete
One sample, and utilizing the method spectral scan number of times is 32 times～64 times, 1 tester 2～just can completely divide for 4 minutes
Analyse a sample, substantially increase work efficiency.And the most do not use any solvent, do not result in secondary dirty
Dye.This method is applicable to the Fourier transform near infrared instrument of different model.
3 with it, carry out simple pre-treatment to sample, gathers sample NIR transmittance spectroscopy, by set up
Model can quickly record the content of hexamethylenamine, to realize the quick analysis to whole process, reaches to ensure end product quality
Purpose.
Accompanying drawing explanation
Fig. 1 represents the black vinegar near infrared light spectrogram (sample cell module) that tem analysis module gathers；
Fig. 2 represents that hexamethylenamine content near-infrared measured value and actual value graph of a relation are concentrated in checking；
Detailed description of the invention
The method of hexamethylenamine content in the near infrared ray hexamethylenamine-acetum of the present invention, is suitable for each
Planting the FT-IR Fourier transform infrared spectrometer of model, the present embodiment instrument is: Thermo-Nicolet company produces
Antaris II type Fourier Transform Near Infrared instrument.Test temperature: room temperature 25 DEG C.
The present invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
One, collect and process the sample containing hexamethylenamine
Collect and process totally 66, sample, being used for modeling, model evaluation and model optimization.Directly weigh the crow of certain mass
Lip river tropine and acetic acid, preparation crow vinegar solution, in crow vinegar system, the mass percentage content of hexamethylenamine is 7%～11%.Entering
During the design of row sample component concentration, it is to avoid be linearly correlated with between concentration of component, thus the information of mistake is avoided to be loaded into model
In.All reagent are commercially available analytical pure commodity, and acetic acid uses distillation pretreatment, and hexamethylenamine is dried before using at 105 DEG C
12 hours.Randomly drawing 50 samples and carry out model foundation as calibration set, remaining sample is as checking collection, and checking collection is not
Participate in modeling, for the accuracy of detection model.
Two, the NIR transmittance spectroscopy collection of illustrative plates of acquisition correction collection sample.
Using tem analysis modular approach to gather spectrum, before test sample, instrument first preheats half an hour.Gather spectrum
Time, be respectively arranged with a position before and after transmission fluid sample cell, above placing testing sample, after put an empty fluid sample
Pipe, as scanning background.By RESULT-Integration software design workflow, carry out spectra collection.
Spectral scan scope: 12000～4000cm-1, indoor scanning temperature 25 DEG C, spectral resolution 8cm-1, scanning times
64 times, each multiple scanning 3 times, carry out continuous scanning collection spectrum, take its averaged spectrum modeling, eliminate to a certain extent with
The impact of chance error difference.The original near infrared light spectrogram gathering crow vinegar system is shown in Fig. 1.
Three, model is set up
The NIR transmittance spectroscopy of calibration set sample is carried out pretreatment, then closes with corresponding hexamethylenamine content
Connection, selects principal component regression method as bearing calibration, sets up the straightening die between NIR transmittance spectroscopy and hexamethylenamine content
Type.Evaluation index according to model: coefficient R2, cross validation mean square deviation (RMSECV) and mean square deviation (RMSEC) are carried out
Comprehensive analysis, determines optimal models.
(1) preprocess method described in uses single order or second-order differential, Norris derivative filters, Savitzky-Golay puts down
One or more methods in cunning, can eliminate instrumental background or the drift impact on signal.
(2) basic thought of principal component regression is exactly the main constituent first obtaining spectrum, resettles sample size and main constituent
Linear correlation, predict the concentration of unknown sample with the linear function set up.
Use principal component regression method to set up crow vinegar solution near infrared spectrum index to refer to hexamethylenamine mass percentage content
Specifically comprising the following steps that of the relational model of mark C
First calibration set light spectrum matrix X (n × k) of crow vinegar solution is decomposed into the apposition sum of k vector, is transformed to one
Individual new main constituent matrix T, it may be assumed that
X=t1p1 T+t2p2 T+t3p3 T+…tkpk T
In formula, n is calibration set sample number, and t is score vector, and p is load vectors (also referred to as main constituent or main gene).?
In optimal models, calibration set sample number is 50, and optimal main cause subnumber k is 10, substitutes into above formula, can obtain
X=t1p1 T+t2p2 T+t3p3 T+…t10p10 T
T=(t1, t2..., t10)
Hereinafter the calibration set light spectrum matrix X for crow vinegar solution is transformed to the concrete formula of orthogonal main constituent matrix T:
1. taking certain column vector x in calibration set light spectrum matrix X is the initial value of t: t=x；
2. p is calculatedT=tTX/tTt；
3. by pTNormalization, pT=pT/||p||；
4. t, t=Xp/p are calculatedTp；
5. compare new t and old t, see and whether meet the condition of convergence.If meeting the condition of convergence, continue step 6., otherwise
Rebound step is 2.；
If the most completing to calculate required main constituent, then stop calculating；Otherwise calculate residual error battle array E:E=X-tpT；
7. replace X with E, return step 1., ask next main constituent.
After calculating, X is i.e. transformed to orthogonal main constituent matrix T=(t1, t2..., t10)。
The orthogonal matrix T obtained with the calibration set light spectrum matrix X principal component analysis of crow vinegar solution, replaces original absorbance to become
Amount X makees linear regression with mass percentage content C of hexamethylenamine in crow vinegar solution, can set up mass percentage content C and light
Relational model between spectrum:
The least square solution of B is:
B=(TTT)-1TTC
C=TB+E
(3) it is the specific formula for calculation of model performance evaluation index below
1. coefficient R2
In formula, CiIt is the theoretical value of sample,It is the predictive value of near infrared spectrum,It is the meansigma methods of sample theoretical value, n
It is calibration set sample number, R2Closer to 1 explanation predictive value with actual value closer to, then the prediction effect of model is the best.
2. internal validation-cross mean square deviation (RMSECV), it was predicted that mean square deviation (RM SEP) and mean square deviation (RMSEC)
N is calibration set sample number, and m is forecast set sample number, and p is main cause subnumber, and RMSECV, RMSEP, RMSEC are the least, say
The predictive ability of bright model is the strongest.
Result shows, when selecting first derivative+Norris-derivative to carry out Pretreated spectra, and the predictability of model
Can preferably, the model performance obtained is optimal.The model parameter of final modeling is shown in Table 1.
The final modeling parameters of table 1
Four, modeling method is assessed
For the accuracy of detection model prediction, using 16 parts of samples remaining in embodiment step () as checking collection,
Model carries out external certificate, and often group sample test 3 times, averages, and the near infrared spectrum of acquisition is pre-with the model built up
Survey hexamethylenamine content, analytical error, evaluation model.
Table 2 uses the error analysis of PCR tem analysis method hexamethylenamine
The testing mean of hexamethylenamine is close with actual value as can be seen from Table 2, and its maximum absolute error is
0.22%, least absolute error is 0.01%, and mean absolute error is 0.10%, it can thus be seen that the accuracy of this method
Higher, the needs of prediction can be met.Fig. 2 indicates checking and concentrates between hexamethylenamine content near-infrared measured value and actual value
Relation.
Five, the quick mensuration of unknown sample hexamethylenamine content
After the model of this method is built up, just hexamethylenamine content in unknown sample can be used for quickly detecting.Collect new
Hexamethylenamine-acetum as unknown sample, gather the NIR transmittance spectroscopy of all unknown samples, built by this method
Vertical model, can directly obtain the content value of hexamethylenamine.
The measurement result using this method 20 samples to additionally collecting is as shown in table 3.
Predicting the outcome of table 3 this method 20 samples to additionally collecting
Six, the extension of model
When the scope of required detection is when 7%～11% concentration range is outer, by increasing the light of other range of concentrations sample
Spectrum, can limit with the detection of extended method.
Concretely comprise the following steps:
1, collect and the sample preparing other concentration range.Points for attention are with reference to embodiment step one.
2, embodiment step 2 is repeated to step 6.
Claims (1)
1. one kind to hexamethylenamine content analysis method in hexamethylenamine-acetum, it is characterised in that: specifically comprise the following steps that
Step one, collect and process sample；Preparation sample be hexamethylenamine mass percentage content be the black Lip river of 7%～11%
Tropine-acetum, when carrying out the design of sample component concentration, should avoid linearly being correlated with between concentration of component；Sample number
No less than 60 parts, randomly choosing wherein more than 50 parts samples and participate in modeling as calibration set, remaining sample is as checking collection；
Step 2, the NIR transmittance spectroscopy of mensuration calibration set sample；Tem analysis module is used to detect, with empty liquid
Sample cell is that background is scanned, and every part of sample parallel gathers 3 times～5 times, gathers spectral scan 32 times～64 times, sampling every time
The averaged spectrum of product parallel acquisition models as the original spectrum of this sample, spectral scan scope: 12000～4000cm-1, spectrum
Resolution 8cm-1；
Step 3, set up model；The NIR transmittance spectroscopy of calibration set sample is carried out pretreatment, then with corresponding Wu Luotuo
Product content is associated；Again by the bearing calibration of principal component regression method, set up NIR transmittance spectroscopy and hexamethylenamine content
Between calibration model；Evaluation index according to model: correlation coefficient, cross validation mean square deviation and mean square deviation carry out total score
Analysis, determines optimal models.
X=t1p1 T+t2p2T+t3p3 T+…tkpk T
T=Xp/pTp
K=10 in optimal models, T=(t1, t2..., t10)
Least square solution B=(the T of BTT)-1TTC
C=TB+E
X is the calibration set light spectrum matrix of crow vinegar solution, and T is the orthogonal matrix that X principal component analysis obtains, and C is hexamethylenamine quality
Degree index, B is coefficient matrix, and E is residual matrix, and t is score vector, p be load vectors (also referred to as main constituent or
Main gene).In optimal models, calibration set sample number is 50, and optimal main cause subnumber k is 10.
During described preprocess method uses single order or second-order differential, the filtering of Norris derivative, Savitzky-Golay smooth
One or more methods；
Step 4, employing checking collection sample are predicted and evaluate optimal models；The NIR transmittance spectroscopy of each checking collection sample is surveyed
Try at least 3 times, average and carry out hexamethylenamine content analysis, analytical error, evaluation model；
Step 5, the quick of hexamethylenamine content of unknown sample measure；Collect new hexamethylenamine-acetum as the unknown
Sample, gathers the NIR transmittance spectroscopy of all unknown samples, the model set up by step 3, it is possible to directly obtain Wu Luotuo
The content value of product.
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| CN115791694A (en) * | 2022-12-02 | 2023-03-14 | 北京理工大学 | Method for predicting concentration of urotropine in urotropine-acetic acid solution |
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