CN106872398A - A kind of HMX explosives moisture method for fast measuring - Google Patents
A kind of HMX explosives moisture method for fast measuring Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 57
- 239000002360 explosive Substances 0.000 title claims abstract description 40
- 238000001228 spectrum Methods 0.000 claims abstract description 25
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 21
- 238000012545 processing Methods 0.000 claims description 24
- 238000009499 grossing Methods 0.000 claims description 13
- 238000012937 correction Methods 0.000 claims description 11
- 238000010998 test method Methods 0.000 claims description 9
- 238000010606 normalization Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 2
- 230000008020 evaporation Effects 0.000 claims 2
- 230000002265 prevention Effects 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000010238 partial least squares regression Methods 0.000 abstract description 7
- 238000004611 spectroscopical analysis Methods 0.000 abstract description 7
- 238000004806 packaging method and process Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
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- 238000009659 non-destructive testing Methods 0.000 abstract description 2
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- 238000004458 analytical method Methods 0.000 description 14
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- 238000005516 engineering process Methods 0.000 description 11
- 239000002351 wastewater Substances 0.000 description 9
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- 239000000463 material Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000007689 inspection Methods 0.000 description 5
- 238000002512 chemotherapy Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
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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
- 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
- G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
-
- 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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Abstract
The invention discloses a kind of HMX explosives moisture method for fast measuring, including：The HMX explosive samples of different in moisture content are configured, moisture is determined；Gather the near infrared spectrum of HMX explosive samples；Calibration model is set up using PLS after spectroscopic data is pre-processed；The near infrared spectrum for gathering sample to be tested is calculated the moisture of sample to be tested by calibration model.The inventive method is easily evaporated for HMX sample reclaimed waters partial volume in test process, causes sample stability poor, the big problem of resultant error, using 1) in sample making course using plastic packaging bag seal arrangement sample.2) taking many parts of same samples carries out near infrared spectrum scanning acquisition averaged spectrum to reduce sample otherness.3) it is modeled using correlation coefficient process selected characteristic wave band.The PLS regression model reliabilities set up are high, prediction effect is good, it is possible to achieve to the quick, accurate of moisture, Non-Destructive Testing in HMX explosives.
Description
Technical field
The present invention relates to HMX explosive component detection fields, a kind of specifically HMX explosives moisture quick detection side
Method.
Background technology
The traditional chemical analysis method analysis major constituents degree of accuracy that the eighties is formed in explosive wastewater industry is high, but analysis
Cycle is long, and human error is big, and for complex system, new formula, the new features product that component is more and content is less then cannot be accurate
Really measurement.Existing explosive wastewater physical and chemical performance analysis method of testing can not meet new explosive wastewater complex system to new parameter test and
The demand of assessment, this situation has injured the exploitation of explosive wastewater new product；It is besides national to explosive wastewater industry in recent years
Technological transformation puts into, and explosive wastewater factory analytical and testing instrument has very fast development, but because method of testing falls behind, it is large quantities of that technological transformation puts into
Analysis Instrument equipment is difficult to performance should be profitable.Therefore the support of the quick analysis test method research of explosive wastewater physicochemical property is increased
Dynamics, lifts industry analysis measuring technology level as early as possible, meets the advanced national defence weapon equipment technology of China and explosive wastewater technology is fast
The need for speed development, with very major and immediate significance.
Near-infrared spectral analysis technology has without pretreatment, is capable of achieving contactless remote detection, and security is good, reliable
The features such as property high and strong ambient adaptability, it is particularly suitable for explosive wastewater Site Detection and on-line analysis, has been applied to various containing energy
Production, monitoring and the inspection of material.
The conventional method of HMX explosive moisture measurements field application is Oven Method, and cycle (nearly 4 hours) long, power consumption are big.This hair
The bright technical problem to be solved is to provide one kind and solves HMX explosives moisture quick and precisely using near-infrared spectral analysis technology
The method of quantitative determination, overcomes the shortcomings of existing method, has very to the quality control in factory's HMX high volume production process
Important meaning.
The content of the invention
The invention provides a kind of HMX explosives moisture method for quick, in HMX explosives moisture it is fast
Fast, lossless, accurate detection, the problems such as solve cumbersome, time-consuming existing detection method, effort.HMX sample reclaimed water partial volumes are easy
Evaporated in test process, cause sample stability poor, the big problem of resultant error, using plastic packaging bag seal arrangement sample, and
Taking many parts of same samples carries out near infrared spectrum scanning acquisition averaged spectrum to reduce sample otherness.Use coefficient correlation simultaneously
Method selected characteristic wave band is modeled, and obtains the more preferable model of prediction effect.
A kind of HMX explosives moisture method for quick, including：
(1) the HMX samples of different in moisture content are prepared, moisture is determined；
(2) gather the near infrared spectrum of HMX explosive samples and pre-processed, HMX samples are set up using PLS
Calibration model in this between moisture and pretreated near infrared spectrum；
(3) gather the near infrared spectrum of sample to be tested and pre-processed, sample to be tested is calculated by calibration model
Moisture；Wherein, the near infrared spectrum scanning wave band 1394.6~1531.8nm of modeling is chosen, 1651.1~
1798.4nm, 1857.3~2010.5nm.
It is the frequency multiplication and combined spectral band of material molecule vibrational spectrum in the range of electromagnetic wavelength 800-2500nm, thus wraps
Contain the abundant information of material composition and molecular structure, can be used for the quantitative determination of component content.Hydric group (O-H) is to light wave
There is very strong absorption, by scanning the near infrared spectrum of sample, the characteristic information of sample reclaimed water molecular radical can be obtained, be used for
Moisture is quantified.
In step (1), described HMX explosives sample selects the product of Baiyin Chemical Industry Group Co., Ltd.Sample
This amount is bigger, and the reliability of constructed model is higher；But sample size crosses conference increases working strength.Described HMX explosive samples
Quantity be preferably more than 80.
In order to build calibration model and be predicted, the 2/3 of total sample can be uniformly extracted as calibration set, remaining is left
1/3 as forecast set, and ensure forecast set uniform concentration distribution, and scope is no more than calibration set.
The method of moisture is determined according to national military standard《GJB772A-1997 explosive test methods》, using chemical method-baking
Dry method.
In step (2), collection near infrared light time spectrum uses optically focused science and technology SupNIR-2750 near-infrared spectrometers, light
Spectral limit：Solid diffusing reflection (1000~2500nm), spectral resolution：≤ 7nm, wavelength accuracy：Better than ± 0.5nm, wavelength
Repeatability：Less than 0.1nm, veiling glare：Less than 0.1%.
In order to reduce spectroscopic data, by collection fashionable dress sample difference, sample be uneven etc., factor brings is influenceed, and described is pre-
Treatment can be using Savitzky-Golay convolution smoothing processing, Savitzky-Golay derivative processings, normalization
(normalization) treatment, multiplicative scatter correction (MSC), baseline correction (baseline) and standard normal variable conversion
(SNV) one or more in.Can be simplified by pretreatment, strengthen model, wherein, S-G smoothing processings are substantially a kind of
Weighted mean method, is to eliminate a kind of the most frequently used method of noise；Normalization is often used to what correction was caused by small light path difference
Spectrum change.MSC is mainly used in eliminating the scattering influence that distribution of particles is uneven and granular size is produced；Baseline correction is mainly used
In the influence for deducting instrumental background or drift about to signal；The purpose of SNV and MSC is essentially identical, is primarily used to eliminate solid
The influence of grain size, surface scattering and change in optical path length to spectrum.
PLS (PLS), PCA (PCR) and ANN can be used when setting up calibration model
One kind in network method (ANN).The present invention can use full spectrum or part modal data, and data using described PLS
Matrix decomposition and return interaction is combined into a step, the feature value vector for obtaining is related to tested component or property, rather than with number
It is related according to the variable for changing maximum in matrix, it is relatively specific for small sample multivariate data analysis, it is possible to use in complicated analysis
System.
Set up during PLS calibration models, checking is interacted by leaving-one method, when checking collection root-mean-square error
(RMSECV) minimum and R is reached2The main gene number used during maximum is considered as optimal.Become them as input
Amount, sets up PLS calibration models, is predicted.
Scanned using all band during collection near infrared spectrum data, spectral scan wave band is 1000~2500nm, is instrument
Full spectral limit parameter can be collected.In order to select the characteristic wave bands comprising effective information, according to the PLS regression coefficients under all band
Figure, characteristic wavelength of wavelength of the coefficient correlation absolute value more than 0.3 required for is set to moisture, and selected wave band is
1394.6~1531.8nm, 1651.1~1798.4nm, 1857.3~2010.5nm.Using this feature wave band, can not only be effective
Improve prediction effect, and can greatly reduce modeling in operand, improve modeling speed, for the exploitation of detecting instrument provide according to
According to.
The quality of model performance is standard with the accurate differentiation rate to forecast set sample, can use prediction related coefficient
R2, prediction mean square deviation (RMSECV), remaining predicted deviation (RPD) evaluation model performance.R2Value is higher, and RMSECV values are smaller, explanation
Model performance is better.Table 1 show the parameter comparison of the correction model after various pretreatments.
Moisture PLS model parameters in the HMX samples of table 1
It can be seen that pretreatment employ S-G (Savitzky-Golay) smoothing processing, S-G derivative processings, at normalization
The model R that reason (normalization), multiplicative scatter correction (MSC) method are set up2It is 0.99995 to be worth, close to 1, explanation
HMX moistures and spectroscopic data have extraordinary correlation, and prediction effect is best；RMSECV values are 0.20208, show model
With good predictive ability.Therefore it is optimal models to select this model.
Fig. 2 shows PRESS values, student's residual error, predicted value-actual value control and the mahalanobis distance value of optimal models.
In order to verify the validity of near infrared spectroscopy, same HMX samples 7 are surveyed with chemical method is parallel with Near-Infrared Absorption Method respectively
It is secondary, draw two groups of experimental datas such as table 2.By statistical principle, checked to two kinds with homogeneity test of variance (F inspections) and t
The result that test method draws is compared, and two methods are investigated in 95% confidence level with this, and veracity and precision is
It is no equivalent.
The two methods of the result of the test of HMX of table 2
By two methods test result, the homogeneous inspection F=S of variance is carried out2 max/S2 min=0.0389/0.0101=3.86
(smaxIt is s1、s2In higher value, sminIt is s1、s2In smaller value)
Look into F value tables, F0.05(fmax,fmin)=F0.05(6,6)=4.28
Because F=3.86 ＜ 4.28, therefore think s1With s2Without significant difference.That is the precision of Near-Infrared Absorption Method and classical chemical method
Degree is equivalent.
Combination with standard deviation
Statistic
Look into t value tables, t95(n1+n2- 2)=t95(12)=2.23
T=1.00 ＜ 2.23, therefore think when confidence level is 95%, Near-Infrared Absorption Method and classical chemical method are poor without conspicuousness
It is different.That is both degrees of accuracy are equivalent.
The present invention has carried out quantitative point to moisture in HMX using near-infrared spectrum analysis combination chemometric techniques
Analysis, it is pre- by S-G smoothing processings, S-G derivative processings, normalized (normalization) and multiplicative scatter correction (MSC)
After processing and selecting specific band, PLS regression model is established.By statistical principle, examined with homogeneity of variance
Test (F inspections) and t inspections be compared to the HMX moisture results that near infrared spectroscopy and chemical drying method are measured, it is believed that
When confidence level is 95%, there was no significant difference for Near-Infrared Absorption Method and classical chemical method, i.e. both degrees of accuracy are equivalent.
The PLS regression model validity set up of the invention is good, reliability is high, estimation range is wide, to be measured
The prediction effect of moisture is good in sample, it is possible to achieve to the quick, accurate of moisture, Non-Destructive Testing in HMX.
Brief description of the drawings
Fig. 1 is full spectrum samples averaged spectrum curve map in embodiment；
Fig. 2 is HMX moisture near-infrared optimal model parameters values in embodiment 4, and (a) (b) (c) (d) is respectively successively PRESS
Value, predicted value-actual value control, mahalanobis distance value and student's residual error；
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1：
1 sample preparation
Preparing 134 HMX samples of different in moisture content is used to set up whole data set.Each sample is placed on unified modeling
In material packaging bag, whole experiment is carried out at 20 ± 2 DEG C of room temperature.
2 use chemical gauging moisture
According to national military standard《GJB772A-1997 explosive test methods》, chemical method-oven drying method carries out the determination of moisture of sample；
Measured value is the content value (g) in 10 grams of samples.Measurement result is shown in Table 3.
2/3 (amounting to 89) of gross sample is uniformly extracted after being ranked up according to moisture measurement value as calibration set, remaining
Remaining 1/3 used as forecast set, it is ensured that forecast set uniform concentration distribution, and scope is no more than calibration set.
Moisture (g/10g) specimen sample number of the modeling of table 3 collection and forecast set
3 PLSs (PLS) based on specific band are modeled
Optically focused science and technology SupNIR-2750 near-infrared spectrometers, spectral region：1000~2500nm, sample state：
Grain or the solid, resolution ratio such as powdered：11 ± 0.3nm at 1529.5nm, wavelength accuracy：<0.2nm, wavelength repeatability：<
0.01nm, absorbance noise：<5×10-5AU.All of chemical measure analysis are performed by The Unscrambler9.8 softwares.
(1) spectral measurement and chemometrics application
The spectrum of each sample is the average value of continuous 30 scanning.The spectral absorbance values of all samples are averaged,
Obtain the curve of spectrum as shown in Figure 1.All spectroscopic datas importing chemo metric software The will be collected to obtain
Unscrambler9.8, obtains the near-infrared primary light spectrogram of sample, and then spectrum is pre-processed, and preprocess method is used
Savitzky-Golay smoothing processings.
(2) wave band modeling is chosen
After through S-G (Savitzky-Golay) smoothing processing, according to the PLS regression coefficient figures under all band, moisture is contained
Amount set the characteristic wavelength required for wavelength of the coefficient correlation absolute value more than 0.3 is, and selected wave band is 1394.6~
1531.8nm, 1651.1~1798.4nm, 1857.3~2010.5nm.Then using PLS method combination cross verifications to school
Positive collection sample sets up calibration model, while making validation-cross, and carries out external certificate, then root to institute's established model with checking collection sample
Determine to obtain final HMX moistures near-infrared forecast model according to the major parameter of near infrared correction.
The quick measure of 4 unknown moisture HMX samples
Unknown moisture HMX samples are taken and fills sample disc in right amount, gather its near infrared spectrum, by spectrum by pre- place
In substituting into the forecast model of foundation after reason, through computing can unknown sample in moisture.
Embodiment 2：
1 sample preparation
Preparing 134 HMX samples of different in moisture content is used to set up whole data set.Each sample is placed on unified modeling
In material packaging bag, whole experiment is carried out at 20 ± 2 DEG C of room temperature.
2 use chemical gauging moisture
According to national military standard《GJB772A-1997 explosive test methods》, chemical method-oven drying method carries out the determination of moisture of sample；
Measured value is the content value (g) in 10 grams of samples.Measurement result is shown in Table 4.
2/3 (amounting to 89) of gross sample is uniformly extracted after being ranked up according to moisture measurement value as calibration set, remaining
Remaining 1/3 used as forecast set, it is ensured that forecast set uniform concentration distribution, and scope is no more than calibration set.
Moisture (g/10g) specimen sample number of the modeling of table 4 collection and forecast set
3 PLSs (PLS) based on specific band are modeled
Optically focused science and technology SupNIR-2750 near-infrared spectrometers, spectral region：1000~2500nm, sample state：
Grain or the solid, resolution ratio such as powdered：11 ± 0.3nm at 1529.5nm, wavelength accuracy：<0.2nm, wavelength repeatability：<
0.01nm, absorbance noise：<5×10-5AU.All of chemical measure analysis are performed by The Unscrambler9.8 softwares.
(1) spectral measurement and chemometrics application
The spectrum of each sample is the average value of continuous 30 scanning.The spectral absorbance values of all samples are averaged,
Obtain the curve of spectrum as shown in Figure 1.All spectroscopic datas importing chemo metric software The will be collected to obtain
Unscrambler9.8, obtains the near-infrared primary light spectrogram of sample, and then spectrum is pre-processed, and preprocess method is used
S-G smoothing processings and S-G derivative processings.
(2) wave band modeling is chosen
After through S-G smoothing processings and S-G derivative processings, according to the PLS regression coefficient figures under all band, moisture is set
Wavelength of the phased relationship number absolute value more than 0.3 is required characteristic wavelength, and selected wave band is 1394.6~1531.8nm,
1651.1~1798.4nm, 1857.3~2010.5nm.Then calibration set sample is built using PLS method combination cross verifications
Vertical calibration model, while making validation-cross, and carries out external certificate, further according to near-infrared school with checking collection sample to institute's established model
The major parameter of positive model determines to obtain final HMX moistures near-infrared forecast model.
The quick measure of 4 unknown moisture HMX samples
Unknown moisture HMX samples are taken and fills sample disc in right amount, gather its near infrared spectrum, by spectrum by pre- place
In substituting into the forecast model of foundation after reason, through computing can unknown sample in moisture.
Embodiment 3：
1 sample preparation
Preparing 134 HMX samples of different in moisture content is used to set up whole data set.Each sample is placed on unified modeling
In material packaging bag, whole experiment is carried out at 20 ± 2 DEG C of room temperature.
2 use chemical gauging moisture
According to national military standard《GJB772A-1997 explosive test methods》, chemical method-oven drying method carries out the determination of moisture of sample；
Measured value is the content value (g) in 10 grams of samples.Measurement result is shown in Table 5.
2/3 (amounting to 89) of gross sample is uniformly extracted after being ranked up according to moisture measurement value as calibration set, remaining
Remaining 1/3 used as forecast set, it is ensured that forecast set uniform concentration distribution, and scope is no more than calibration set.
Moisture (g/10g) specimen sample number of the modeling of table 5 collection and forecast set
3 PLSs (PLS) based on specific band are modeled
Optically focused science and technology SupNIR-2750 near-infrared spectrometers, spectral region：1000~2500nm, sample state：
Grain or the solid, resolution ratio such as powdered：11 ± 0.3nm at 1529.5nm, wavelength accuracy：<0.2nm, wavelength repeatability：<
0.01nm, absorbance noise：<5×10-5AU.All of chemical measure analysis are performed by The Unscrambler9.8 softwares.
(1) spectral measurement and chemometrics application
The spectrum of each sample is the average value of continuous 30 scanning.The spectral absorbance values of all samples are averaged,
Obtain the curve of spectrum as shown in Figure 1.All spectroscopic datas importing chemo metric software The will be collected to obtain
Unscrambler9.8, obtains the near-infrared primary light spectrogram of sample, and then spectrum is pre-processed, and preprocess method is used
S-G smoothing processings, S-G derivative processings and normalized.
(2) wave band modeling is chosen
After through S-G smoothing processings, S-G derivative processings and normalized, according to the PLS regression coefficient figures under all band,
Characteristic wavelength of wavelength of the coefficient correlation absolute value more than 0.3 required for is set to moisture, selected wave band is
1394.6~1531.8nm, 1651.1~1798.4nm, 1857.3~2010.5nm.Then tested with reference to interaction using PLS methods
Demonstration sets up calibration model to calibration set sample, while making validation-cross, and carries out outside to institute's established model with checking collection sample
Checking, the major parameter further according near infrared correction determines to obtain final HMX moistures near-infrared forecast model.
The quick measure of 4 unknown moisture HMX samples
Unknown moisture HMX samples are taken and fills sample disc in right amount, gather its near infrared spectrum, by spectrum by pre- place
In substituting into the forecast model of foundation after reason, through computing can unknown sample in moisture.
Embodiment 4：
1 sample preparation
Preparing 134 HMX samples of different in moisture content is used to set up whole data set.Each sample is placed on unified modeling
In material packaging bag, whole experiment is carried out at 20 ± 2 DEG C of room temperature.
2 use chemical gauging moisture
According to national military standard《GJB772A-1997 explosive test methods》, chemical method-oven drying method carries out the determination of moisture of sample；
Measured value is the content value (g) in 10 grams of samples.Measurement result is shown in Table 6.
2/3 (amounting to 89) of gross sample is uniformly extracted after being ranked up according to moisture measurement value as calibration set, remaining
Remaining 1/3 used as forecast set, it is ensured that forecast set uniform concentration distribution, and scope is no more than calibration set.
Moisture (g/10g) specimen sample number of the modeling of table 6 collection and forecast set
3 PLSs (PLS) based on specific band are modeled
Optically focused science and technology SupNIR-2750 near-infrared spectrometers, spectral region：1000~2500nm, sample state：
Grain or the solid, resolution ratio such as powdered：11 ± 0.3nm at 1529.5nm, wavelength accuracy：<0.2nm, wavelength repeatability：<
0.01nm, absorbance noise：<5×10-5AU.All of chemical measure analysis are performed by The Unscrambler9.8 softwares.
(1) spectral measurement and chemometrics application
The spectrum of each sample is the average value of continuous 30 scanning.The spectral absorbance values of all samples are averaged,
Obtain the curve of spectrum as shown in Figure 1.All spectroscopic datas importing chemo metric software The will be collected to obtain
Unscrambler9.8, obtains the near-infrared primary light spectrogram of sample, and then spectrum is pre-processed, and preprocess method is used
S-G smoothing processings, S-G derivative processings, normalized and MSC methods.
(2) wave band modeling is chosen
After being processed through S-G smoothing processings, S-G derivative processings, normalized and MSC methods, according to the PLS under all band
Regression coefficient figure, characteristic wavelength of wavelength of the coefficient correlation absolute value more than 0.3 required for is set to moisture, selected
Wave band is 1394.6~1531.8nm, 1651.1~1798.4nm, 1857.3~2010.5nm.Then combined using PLS methods
Cross verification sets up calibration model to calibration set sample, while making validation-cross, and institute's established model is entered with checking collection sample
Row external certificate, the major parameter further according near infrared correction determines to obtain final HMX moistures near-infrared prediction mould
Type.
The quick measure of 4 unknown moisture HMX samples
Unknown moisture HMX samples are taken and fills sample disc in right amount, gather its near infrared spectrum, by spectrum by pre- place
In substituting into the forecast model of foundation after reason, through computing can unknown sample in moisture.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to model of the invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, those skilled in the art make to technical scheme
The various modifications for going out and improvement, all should fall into the protection domain of claims of the present invention determination.
Claims (6)
1. a kind of HMX explosives moisture method for fast measuring, including：
(1) the HMX samples of different in moisture content are prepared, according to national military standard《GJB772A-1997 explosive test methods》Determine sample
Moisture；
(2) gather the near infrared spectrum of HMX explosive samples and pre-processed, set up in HMX samples using PLS
Calibration model between moisture and pretreated near infrared spectrum.Wherein, the near infrared spectrum scanning ripple of modeling is chosen
Section 1394.6~1531.8nm, 1651.1~1798.4nm, 1857.3~2010.5nm.
(3) gather the near infrared spectrum of sample to be tested and pre-processed, the water of sample to be tested is calculated by calibration model
Divide content.
2. HMX explosives moisture method for quick according to claim 1, it is characterised in that described HMX explosives
Water content of the sample content range is more than 80 for the quantity of 0.3~30%, HMX explosive samples.
3. HMX explosives moisture method for quick according to claim 1, it is characterised in that in step (1), be
Prevent moisture evaporation from changing the method for employing the sealing of electrostatic prevention plastic envelope.
4. HMX explosives moisture method for quick according to claim 1, it is characterised in that in step (1), surveys
The method for determining moisture is the Oven Method of GJB772A-1997-102.1,100 DEG C of oven temperature, drying time 1h, it is allowed to poor
0.01%.
5. HMX explosives moisture method for quick according to claim 1, it is characterised in that step (2) or (3)
In, described preprocess method uses Savitzky-Golay convolution smoothing processing, Savitzky-Golay derivative processings, normalizing
Change treatment (normalization), multiplicative scatter correction (MSC).
6. HMX explosives moisture method for quick according to claim 1, it is characterised in that step (2) or (3)
In, described collection sample to be tested near infrared spectrum carries out near infrared spectrum scanning and obtains flat using taking more than 3 parts of same samples
Equal spectrum is reduced because of the sample otherness that moisture evaporation causes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108663340A (en) * | 2018-07-31 | 2018-10-16 | 甘肃畅陇公路养护技术研究院有限公司 | A kind of measurement method and system of sand moisture content |
| CN111579525A (en) * | 2020-05-15 | 2020-08-25 | 甘肃银光化学工业集团有限公司 | Device for automatically detecting moisture of powdery energetic material |
| CN114441469A (en) * | 2022-02-24 | 2022-05-06 | 龙岩烟草工业有限责任公司 | Calibration method and device of moisture meter and computer equipment |
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| CN105277508A (en) * | 2015-11-24 | 2016-01-27 | 泸州北方化学工业有限公司 | Near-infrared detection method for moisture content of nitrocotton |
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| CN104897595A (en) * | 2015-05-21 | 2015-09-09 | 四川大学 | Method for simultaneously measuring contents of HMX, RDX and TNT in PBX explosive by ultraviolet spectrometry |
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| CN108663340A (en) * | 2018-07-31 | 2018-10-16 | 甘肃畅陇公路养护技术研究院有限公司 | A kind of measurement method and system of sand moisture content |
| CN111579525A (en) * | 2020-05-15 | 2020-08-25 | 甘肃银光化学工业集团有限公司 | Device for automatically detecting moisture of powdery energetic material |
| CN111579525B (en) * | 2020-05-15 | 2023-10-20 | 甘肃银光化学工业集团有限公司 | Device for automatically detecting water content of powdery energetic material |
| CN114441469A (en) * | 2022-02-24 | 2022-05-06 | 龙岩烟草工业有限责任公司 | Calibration method and device of moisture meter and computer equipment |
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