CN108827907A - It is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration - Google Patents
It is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 67
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 25
- 238000003556 assay Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000005259 measurement Methods 0.000 claims abstract description 21
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- 239000000126 substance Substances 0.000 claims abstract description 10
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- 239000000523 sample Substances 0.000 claims description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000001228 spectrum Methods 0.000 claims description 20
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- 244000146553 Ceiba pentandra Species 0.000 claims description 16
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000835 fiber Substances 0.000 claims description 9
- 239000012488 sample solution Substances 0.000 claims description 9
- 239000011550 stock solution Substances 0.000 claims description 9
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 claims description 8
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- 238000005457 optimization Methods 0.000 claims description 3
- 238000010238 partial least squares regression Methods 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
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- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012895 dilution Substances 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
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- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 2
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- 238000009395 breeding Methods 0.000 description 2
- 230000001488 breeding effect Effects 0.000 description 2
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 2
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- 239000011591 potassium Substances 0.000 description 2
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- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
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- 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
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Abstract
The present invention relates to a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration, this method is completed by the model prediction step of sample acquisition, the acquisition of near-infrared spectrogram, sweep parameter setting, the measurement of sample chemical chromatic value, spectroscopic data pretreatment, the foundation of calibration model and sample chromatic value content, this method is without pre-processing sample, it is convenient and efficient, there is no any side effect to human body and environment, testing result relative deviation is small, if the chemical measurements precision of test sample is high, predicted value of the invention if, can be close to true value.This method quickly detected solves color cotton in popularization and purchases, the key technical problems such as quality identification and classification in processing link, entire near infrared detection process only needs short a few minutes, have the characteristics that easy to operate, detection is quick, determination efficiency is high, is worth promoting and applying in color cotton is chosen and identifies.
Description
Technical field
The present invention relates to the technical fields of Xinjiang color cotton colorimetric detection, more particularly to one kind to pass through near infrared technology pair
The rapid assay methods of brown coloured silk cotton chromatic value.
Background technique
Natural colored color cotton is that a kind of fiber in cotton boll blowing cultivated using modern biotechnology is just had
The fabric raw material of natural colour.Natural colored coloured silk cotton has the characteristics that nature is soft, simple and tasteful, and fiber after cleaning
Textile color can also gradually deepen, and without harmful substances such as formaldehyde, azo dyes in textile, and have antistatic, stop
The function of itching is disturbed, is qualified " green product ", is known as " biological garments ".Color cotton has kind in the numerous areas in the whole nation
It plants, extremely important effect has been played in the textile industry in China.
Not only its fiber quality is identified in choosing in work for color cotton, be seemed to the chromaticity evaluation classification of color cotton
It is even more important.Currently, traditional color cotton fiber classifier relies primarily on artificial eye observation to analyze color, so
And the difference of 2 colors can only be visually differentiated, and absolute measurement cannot be carried out to color.In addition, color cotton color is vulnerable to light
According to the influence of condition, when external light source changes, the colour generation of color cotton also can accordingly change, this distinguishes and comment to visually measurement
Valence coloured silk cotton color grade etc. brings very big interference.Later, China mostly used international color model to the detection of color cotton color
(CIELAB) textile chromascope is measured, and is also had and is carried out colour measurement based on HVI cotton detecting large volume instrument.However,
Some researches show that the laboratory spectrophotometers using modernization establish conventional H VI color system (using Rd and+b parameter) and
When the system of CIELAB, analyzer is lower to the measurement degree of correlation of cotton-wool, and cotton fiber color is vulnerable to porcelain plate color grading
Etc. the influence of objective factors and generate deviation.Therefore, a kind of accurate, the quickly color cotton coloration of measurement method is found out, to color cotton product
Quality Control fixture is significant.
Summary of the invention
Present invention aims at provide a kind of rapid assay methods based near infrared spectrum to color cotton coloration, this method
Be by sample acquisition, the acquisition of near-infrared spectrogram, sweep parameter setting, sample chemical chromatic value measurement, spectroscopic data pretreatment,
The foundation of calibration model and the model prediction step of sample chromatic value content are completed, and this method is not necessarily to pre-process sample,
It is convenient and efficient, there is no any side effect to human body and environment, testing result relative deviation is small, the chemical measurements essence of test sample
Degree is high, and predicted value of the invention then can be close to true value.This method quickly detected solves color cotton in a large amount of breeding materials
The screening and popularization of material, the key technical problems such as quality identification and classification in the purchase of color cotton raw material, processing link are entire close red
Outer detection process only needs short a few minutes, has the characteristics that easy to operate, detection is quick, determination efficiency is high, is worth selecting in color cotton
It is promoted and applied in purchase identification.
It is of the present invention it is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration, follow these steps into
Row:
Sample acquisition:
A, acquisition mature various strains, various maturity periods and the drying at each position brown coloured silk cotton sample product, will adopt respectively
The brown color cotton fiber sample of collection dries, and removes cottonseed, sawdust impurity, is allowed to that colour generation is uniform, is stored in dry brown paper letter
It is spare in envelope;
The acquisition of sample near-infrared spectrogram:
B, it is acquired using the rotation diffusing reflection sampling system of near infrared spectrometer, preheats nir instrument before test
30min selects brown to have 150 parts of color region representativeness brown color cotton fiber, and is numbered, precise 1.0g brown
Cotton fiber sample is placed in rotating sample pool, and using background built in instrument as reference, using Rotating with Uniform mode, it is closely red to obtain sample
External spectrum figure, twice, sampling area is not exclusively overlapped each Sample Scan;
Sweep parameter setting:
C, spectra collection range 1000nm-2400nm, scanning times 32 times, resolution ratio 32cm-1, scanning temperature is 20 DEG C, wet
Degree is 35%, after acquisition, and taking sample averaged spectrum is the final spectrum of sample;
The measurement of sample chemical chromatic value:
D, the brown cotton fiber 1.0g after taking step c to acquire, the sodium hydroxide solution 50mL for being 1% with mass fraction are super
Sound extracts 2 times, and combined extract supplies weightlessness, uses 0.5molL-1Hydrochloric acid solution adjusts extracting solution pH=7, as sample
Product solution;
E, color standard stock solution, standard are prepared according to platinum-cobalt method in the measuring method of GB11903-89 water quality coloration
The chromatic value of serial solution and measurement Cotton Fiber of Natural Brown Cotton sample;
Sample classification:
F, in near-infrared measurement software, by the primary light of the chromatic value of obtained measurement Cotton Fiber of Natural Brown Cotton sample and acquisition
Spectrum corresponds to each other, and is uniformly distributed principle according to calibration set sample, and sample sets are divided into calibration set and verifying collects, specific method:It is first
Obtained representative brown color cotton fiber chromatic value is ranked up from small to large first, then takes 1 to be used as verifying every 5
Collection, remaining adjusts the minimum value and maximum value of brown color cotton fiber chromatic value as calibration set, is allowed to incorporate into as correction
Collection, calibration samples collection and verifying sample set are used to establish quantitative calibration models, and forecast sample collection is used to the accuracy of detection model
And repeatability, wherein calibration set sample content is 60%, and calibration samples collection content is 20%, and forecast sample collection content is 20%;
The foundation and optimization of model:
G, the importing SupNIR 2700 of the atlas of near infrared spectra of calibration set sample and the chromatic value of calibration set sample is close red
In the model management interface of external spectrum instrument software, firstly, being carried out in full spectral limit to the near infrared spectrum of calibration set sample pre-
Processing, sample spectral data effectively eliminate the interference of baseline and other backgrounds, improve point by Savitzky-Golay processing
Resolution and sensitivity then establish prediction straightening die to calibration set sample using partial least-squares regression method combination validation-cross
Type optimizes prediction calibration model according to the parameter of near-infrared quantitative calibration models, wherein model near-infrared by changing
Spectral band and spectral manipulation mode optimize processing:Fiber sample is eliminated using multiplicative scatter correction and baseline correction
Surface particles size and fiber surface scatter the influence to spectrogram, optimize map, pass through calibration set standard deviation, validation-cross collection
Standard deviation, forecast set standard deviation and the related coefficient with reference to quantitative calibration models calibration set predicted value and measured value, comprehensive selection
Calibration set standard deviation, validation-cross collection standard deviation are minimum, and quantitative correction collection model and forecast set model related coefficient are maximum, select
Spectral band is that 1 050-1699nm, 1 799-2 399nm carry out establishing calibration model, the model, that is, brown color cotton fiber coloration
It is worth optimal quantitative calibration models;
The prediction of color cotton fiber chromatic value:
H, the brown coloured silk cotton forecast set sample in the classification of selection sample, determines what the importing of its near infrared spectrum data was established
It measures in model, is analyzed by model calculation, it is predicted value that forecast set sample chromatic value, which can be obtained, by predicted value and practical measurement
Value carries out statistical errors analysis, which answers<0.5.
It is of the present invention it is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration, in this method step e
According in the measuring method of GB11903-89 water quality coloration platinum-cobalt method prepare color standard stock solution, standard serial solution and
Measure the chromatic value of Cotton Fiber of Natural Brown Cotton sample;Precise 0.311 ± 0.001g chlordene platinum (IV) (K2PtCl6) acid potassium and 0.250
± 0.001g CoCL2 6H2O (II) (CoCl2·6H2O it) is dissolved in 25mL water, adds 25mL hydrochloric acid 1.18gmL-1, and
Graticule is diluted to deionized water in the volumetric flask of 250mL and obtains the platinum cobalt color standard stock solution that coloration is 500 degree, at one group
In the volumetric flask of 250ml, 2.50,5.00,7.50,10.00,12.50,15.00,17.50,20.00 are separately added into pipette,
30.00 and 35.00 platinum cobalt color standard stock solutions, and with optics pure water (by 0.2um filter membrane in 100ml distilled water or deionization
1h is impregnated in water water, distilled water or deionized water is filtered with it, discards initial 250ml, it is molten to prepare whole standards with this water
Liquid and as dilution water) be diluted to graticule, which is respectively:5,10,15,20,25,30,35,40,50,
60 and 70 degree;
Determination of colority:It by one group of 50ml color-comparison tube, is rushed with color standard solution to graticule, by another group of 50ml tool plug
The test sample solution of the effective step d of colorimetric is rushed to graticule, and color-comparison tube is placed in white surface, colorimetric cylinder and the surface
It should be in suitable angle, reflect light from color-comparison tube bottom upwardly through fluid column.Fluid column is observed vertically downward, is found out
With the immediate standard solution of test sample solution coloration.Such as test sample solution coloration >=70 degree, after the dilution of optics pure water,
Coloration is fallen among standard solution range to be measured.Test sample solution is separately taken to measure Ph value;
Coloration result indicates:The coloration of sample is indicated with the angle value of immediate color standard solution therewith, at 0~40 degree
In the range of (not including 40 degree), it is accurate to 5 degree;Within the scope of 40~70 degree, it is accurate to 10 degree;The sample coloration diluted
(A0), in terms of degree, calculated with following formula:A0=V1/V0×A1
In formula:V1Volume after sample dilution, ml;
V0Volume before sample dilution, ml;
A1The observed value of dilute sample coloration, degree.
It is of the present invention it is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration, the beneficial effect of this method
Fruit:
Compared with prior art, the present invention provides the coloration values determination method of brown color cotton fiber a kind of based on close red
The brown coloured silk cotton chromatic value of external spectrum technology measures prediction model, on the basis of the measurement of known a large amount of sample real contents,
The atlas of near infrared spectra of sample is acquired, the quantitative analysis based on near-infrared spectrum technique and chemistry in detecting is established and predicts mould
Then brown coloured silk cotton sample product to be measured only need to be handled to obtain clean cotton fiber and can be measured, before removing by type by removal of impurities
Phase establishes outside prediction model, and entire near infrared detection process only needs short a few minutes, with easy to operate, detection is quick, measurement
The features such as high-efficient.
In addition, detection method of the invention does not have to any organic solvent, simple physical removal of impurities processing only need to be carried out, to environment
With testing staff without appointing dye and injury, more safety and environmental protection, to brown color cotton fiber choose and breeding work has important meaning
Justice.
Detailed description of the invention
Fig. 1 is the atlas of near infrared spectra that the near infrared spectrum of calibration set sample in present example models after the pre-treatment;
Fig. 2 is cross validation standard deviation S ECV, calibration set coefficient of determination R in present example2With principal component dimension
Variation diagram;
Fig. 3 is the dependency graph in present example between the chromatic value and measured value of forecast set sample.
Specific embodiment
It is right combined with specific embodiments below in order to make those skilled in the art more fully understand technical solution of the present invention
The present invention is described in further detail.The following examples are only intended to illustrate the technical solution of the present invention more clearly, but not
It can be limited the scope of the invention with this.
Embodiment
Sample acquisition:
A, acquisition mature various strains, various maturity periods and the drying at each position brown coloured silk cotton sample product, will adopt respectively
The brown coloured silk cotton sample product of collection are dried, removal cottonseed, the impurity such as sawdust, are allowed to that colour generation is uniform, are stored in dry brown paper
It is spare in envelope;
The acquisition of sample near-infrared spectrogram:
B uses the rotation diffusing reflection sampling system of Chinese 2700 near infrared spectrometer of optically focused Science and Technology Ltd. SupNIR
It is acquired, nir instrument is preheated into 30min before test, select brown that there is color region representativeness brown color cotton fiber
150 parts, and be numbered, precise 1.0g Cotton Fiber of Natural Brown Cotton sample is placed in rotating sample pool, is with background built in instrument
Reference obtains sample atlas of near infrared spectra using Rotating with Uniform mode, each Sample Scan twice, the endless full weight of sampling area
It closes;
Sweep parameter setting:
C, spectra collection range 1000nm-2400nm, scanning times 32 times, resolution ratio 32cm-1, scanning temperature is 20 DEG C, wet
Degree is 35%, after acquisition, and taking sample averaged spectrum is the final spectrum of sample, the near infrared spectrum of 150 batches of samples such as Fig. 1
Shown, abscissa is wavelength (nm), and ordinate is (A);
The measurement of sample chemical chromatic value:
D, the brown cotton fiber 1.0g after taking step c to acquire, the sodium hydroxide solution 50mL for being 1% with mass fraction are super
Sound extracts 2 times, and combined extract supplies weightlessness, uses 0.5molL-1Hydrochloric acid solution adjusts extracting solution pH=7, as sample
Product solution;
E, color standard stock solution, standard are prepared according to platinum-cobalt method in the measuring method of GB11903-89 water quality coloration
The chromatic value of serial solution and measurement Cotton Fiber of Natural Brown Cotton sample;
The preparation of color standard stock solution and standard solution:Precise 0.311 ± 0.001g chlordene platinum (IV)
(K2PtCl6) sour potassium and 0.250 ± 0.001g CoCL2 6H2O (II) (CoCl2·6H2O it) is dissolved in 25mL water, adds 25mL hydrochloric acid
1.18g·mL-1, and be diluted to graticule with deionized water in the volumetric flask of 250mL and obtain the platinum cobalt color scale that coloration is 500 degree
Quasi- stock solution;In the volumetric flask of one group of 250ml, 2.50,5.00,7.50,10.00,12.50 are separately added into pipette,
15.00,17.50,20.00,30.00 and 35.00 platinum cobalt color standard stock solutions, and (0.2um filter membrane is existed with optics pure water
1h is impregnated in 100ml distilled water or deionized water water, distilled water or deionized water is filtered with it, discards initial 250ml, use this
Kind water prepares whole standard solution and as dilution water) it is diluted to graticule.The standard serial solution coloration is respectively:5,10,15,
20,25,30,35,40,50,60 and 70 degree;
Determination of colority:It by one group of 50ml color-comparison tube, is rushed with color standard solution to graticule, by another group of 50ml tool plug
The test sample solution of the effective step d of colorimetric is rushed to graticule, and color-comparison tube is placed in white surface, colorimetric cylinder and the surface
It should be in suitable angle, reflect light from color-comparison tube bottom upwardly through fluid column, observe fluid column vertically downward, find out
With the immediate standard solution of test sample solution coloration, such as test sample solution coloration >=70 degree, after the dilution of optics pure water,
Coloration is fallen among standard solution range to be measured.Test sample solution is separately taken to measure Ph value;
Coloration result indicates:The coloration of sample is indicated with the angle value of immediate color standard solution therewith, in 0-40 degree
In the range of (not including 40 degree), it is accurate to 5 degree;Within the scope of 40-70 degree, it is accurate to 10 degree;Sample coloration (the A diluted0),
In terms of degree, calculated with following formula:A0=V1/V0×A1
In formula:V1Volume after sample dilution, ml;
V0Volume before sample dilution, ml;
A1The observed value of dilute sample coloration, degree;
Sample classification:
F, the original spectrum of the sample determination of colority value that sample is obtained in step e and acquisition is corresponded to each other, according to correction
Collection sample is uniformly distributed principle, and sample sets are divided into calibration set and verifying collects, and calibration samples collection and verifying sample set are used to establish
Quantitative calibration models, forecast sample collection are used to the accuracy and repeatability of detection model, wherein calibration set sample content is
60%, calibration samples collection content is 20%, and forecast sample collection content is 20%;
Final selection chromatic value range is calibration set for 84 samples in 5.1-19.2;Chromatic value range is in 5.1-
19.2 64 samples are calibration set, and 2 samples are verifying collection, chromatic value range 5.3-18.6, calibration set and verifying collection
Chromatic value is shown in Table 1 in sample;
The color cotton chromatic value statistical result of table 1
The foundation and optimization of model:
G, the importing SupNIR 2700 of the atlas of near infrared spectra of calibration set sample and the chromatic value of calibration set sample is close red
In the model management interface of external spectrum instrument software, firstly, being carried out in full spectral limit to the near infrared spectrum of calibration set sample pre-
Processing, sample spectral data effectively eliminate the interference of baseline and other backgrounds, improve point by Savitzky-Golay processing
Resolution and sensitivity then establish prediction straightening die to calibration set sample using partial least-squares regression method combination validation-cross
Type optimizes prediction calibration model according to the parameter of near-infrared quantitative calibration models, wherein model near-infrared by changing
Spectral band and spectral manipulation mode optimize processing:Using multiplicative scatter correction (Multiplicative scatter
Correction, MSC) and baseline correction (Baseline correction, BLC) eliminate fiber sample surface particles size with
And the influence of fiber surface scattering and change in optical path length to spectrogram, smooth, continuous spectrogram (Fig. 1) is finally obtained, such as Fig. 1 institute
Show, in the SPECTRAL REGION of 1 000-2 400nm of wavelength, the near infrared light spectral curve of sample show many places absorption peak be incremented by or
The trend successively decreased illustrates that test brown coloured silk cotton sample used originally has good spectral response in this area, meanwhile, different samples
Its near infrared light spectral curve is similar but is not exclusively overlapped, and embodies the otherness and continuity between sample;
It is corrected by calibration set standard deviation, validation-cross collection standard deviation, forecast set standard deviation and reference quantitative calibration models
Collect the related coefficient of predicted value and measured value, comprehensive selection calibration set standard deviation, validation-cross collection standard deviation are minimum, quantitative correction
Collection model and forecast set model related coefficient are maximum, select spectral band for 1 050-1 699nm, 1 799-2 399nm progress
Calibration model is established, the model, that is, optimal quantitative calibration models of brown color cotton fiber chromatic value, according to the model, model is determined
Determine coefficient be 0.984, calibration SEC be 0.638, SECV 0.813, number of main factor 10, to spectrum file carry out cross validation,
Obtain prediction residual quadratic sum (Prediction residual error sum of squares, PRESS) value of the spectrum
With the tendency chart (Fig. 2) changed by subnumber;
The prediction of color cotton fiber chromatic value:
H, after the completion of model foundation, it is the accuracy and stability for further verifying the model, randomly chooses 20 parts of step f
In brown coloured silk cotton forecast set sample, 20 parts of forecast set sample near infrared spectrum datas are imported in established quantitative model,
It is analyzed by model calculation, it is predicted value that forecast set sample chromatic value, which can be obtained, and predicted value and actual measured value are united
Meter learns error analysis, which answers<0.5 is shown in Table 2;
2 model of table is to forecast set sample chromatic value prediction result
By prediction result as it can be seen that model external prediction deviation≤0.5, standard deviation 0.310 shows the model pair
The prediction of brown coloured silk cotton chromatic value is accurate;
Contrast table 1 is as can be seen that the chromatic value variation range of external certificate collection (forecast set) sample is no more than calibration set sample
The range of product.By the prediction result in table 2 it is found that forecast set sample chromatic value is with chemical measurements (true value) related coefficient
0.984, SEC 0.468, SECV 0.516.Actual prediction to model built is the results show that chromatic value predicts average deviation
It is -0.1553, predicted value standard deviation is 0.589, error range -0.3~0.5, from the figure 3, it may be seen that utilizing near infrared spectrum pair
There are good linear relationship between the predicted value and chemical measurements (true value) of brown coloured silk cotton sample product coloration, correlation is aobvious
It writes, shows that using chromatic value in this method analysis brown color cotton fiber be feasible;
The prediction stability of quantitative calibration models:
To verify quantitative model stability, Z1456 sample is randomly selected, multiple scanning spectrogram 10 times, and measure it
Scanning optical spectrum figure is updated in established model by chromatic value, obtains the prediction result of corresponding chromatic value, and examines quantitative mould
Type stability result is shown in Table 3;
3 quantitative model stability test result of table
As can be seen from the table:Predict that sample standard deviation is 0.31, relative standard deviation 2.2%, it was demonstrated that this is quantitative
Model stability is reliable, precision with higher, can satisfy the requirement of brown coloured silk cotton chromatic value fast quantitative analysis.
Claims (1)
1. it is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration, it is characterised in that follow these steps to carry out:
Sample acquisition:
A, acquisition mature various strains, various maturity periods and the drying at each position brown coloured silk cotton sample product, respectively by acquisition
Brown color cotton fiber sample dries, and removes cottonseed, sawdust impurity, is allowed to that colour generation is uniform, is stored in dry kraft envelope
It is spare;
The acquisition of sample near-infrared spectrogram:
B, it is acquired using the rotation diffusing reflection sampling system of near infrared spectrometer, nir instrument is preheated 30 before test
Min selects brown to have 150 parts of color region representativeness brown color cotton fiber, and is numbered, precise 1.0g brown cotton
Fiber sample is placed in rotating sample pool, using background built in instrument as reference, using Rotating with Uniform mode, obtains sample near-infrared
Spectrogram, twice, sampling area is not exclusively overlapped each Sample Scan;
Sweep parameter setting:
C, spectra collection range 1000nm-2400nm, scanning times 32 times, resolution ratio 32cm-1, scanning temperature is 20 DEG C, wet
Degree is 35%, after acquisition, and taking sample averaged spectrum is the final spectrum of sample;
The measurement of sample chemical chromatic value:
D, 1.0 g of brown cotton fiber after taking step c to acquire, the sodium hydroxide solution 50 mL ultrasound for being 1% with mass fraction
It extracts 2 times, combined extract supplies weightlessness, with 0.5 molL-1Hydrochloric acid solution adjusts extracting solution pH=7, as test sample
Solution;
E, color standard stock solution, standard series are prepared according to platinum-cobalt method in the measuring method of GB11903-89 water quality coloration
The chromatic value of solution and measurement Cotton Fiber of Natural Brown Cotton sample;
Sample classification:
F, in near-infrared measurement software, by the original spectrum phase of the chromatic value of obtained measurement Cotton Fiber of Natural Brown Cotton sample and acquisition
It is mutually corresponding, it is uniformly distributed principle according to calibration set sample, sample sets are divided into calibration set and verifying collects, specific method:First will
Obtained representative brown color cotton fiber chromatic value is ranked up from small to large, then takes 1 to collect as verifying every 5,
It is remaining to be used as calibration set, and the minimum value and maximum value of brown color cotton fiber chromatic value are adjusted, it is allowed to incorporate into as calibration set, correction
Sample set and verifying sample set are used to establish quantitative calibration models, and forecast sample collection is used to the accuracy and repetition of detection model
Property, wherein calibration set sample content is 60%, and calibration samples collection content is 20%, and forecast sample collection content is 20%;
The foundation and optimization of model:
G, by 2700 near infrared light of importing SupNIR of the atlas of near infrared spectra of calibration set sample and the chromatic value of calibration set sample
In the model management interface of spectrometer software, firstly, the near infrared spectrum of calibration set sample is pre-processed in full spectral limit,
Sample spectral data is handled by Savitzky-Golay, is effectively eliminated the interference of baseline and other backgrounds, is improved resolution ratio
And sensitivity, prediction calibration model, root are then established to calibration set sample using partial least-squares regression method combination validation-cross
Prediction calibration model is optimized according to the parameter of near-infrared quantitative calibration models, wherein model near infrared spectrum by changing
Wave band and spectral manipulation mode optimize processing:Fiber sample surface is eliminated using multiplicative scatter correction and baseline correction
Granular size and fiber surface scatter the influence to spectrogram, optimize map, pass through calibration set standard deviation, validation-cross collection mark
Quasi- poor, forecast set standard deviation and the related coefficient with reference to quantitative calibration models calibration set predicted value and measured value, comprehensive selection school
Positive collection standard deviation, validation-cross collection standard deviation are minimum, and quantitative correction collection model and forecast set model related coefficient are maximum, select light
Spectrum wave band is that 1050-1699nm, 1799-2399 nm carry out establishing calibration model, and the model, that is, brown color cotton fiber chromatic value is most
Excellent quantitative calibration models;
The prediction of color cotton fiber chromatic value:
H, the brown coloured silk cotton forecast set sample in step f is selected, its near infrared spectrum data is imported to established quantitative model
In, it is analyzed by model calculation, it is predicted value that forecast set sample chromatic value, which can be obtained, and predicted value and actual measured value are carried out
Statistical errors analysis, the model external prediction result relative standard deviation are answered<0.5.
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