CN108061724A - The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum - Google Patents

The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum Download PDF

Info

Publication number
CN108061724A
CN108061724A CN201711267876.2A CN201711267876A CN108061724A CN 108061724 A CN108061724 A CN 108061724A CN 201711267876 A CN201711267876 A CN 201711267876A CN 108061724 A CN108061724 A CN 108061724A
Authority
CN
China
Prior art keywords
calibration
sample
coloured silk
cotton
quantitative
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711267876.2A
Other languages
Chinese (zh)
Inventor
阿依古丽·塔什博拉提
李慕春
方智三
宋良辉
韩飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
XINJIANG UYGUR AUTONOMOUS REGION INSTITUTE FOR INSTRUMENTAL ANALYSIS
Original Assignee
XINJIANG UYGUR AUTONOMOUS REGION INSTITUTE FOR INSTRUMENTAL ANALYSIS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by XINJIANG UYGUR AUTONOMOUS REGION INSTITUTE FOR INSTRUMENTAL ANALYSIS filed Critical XINJIANG UYGUR AUTONOMOUS REGION INSTITUTE FOR INSTRUMENTAL ANALYSIS
Priority to CN201711267876.2A priority Critical patent/CN108061724A/en
Publication of CN108061724A publication Critical patent/CN108061724A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light

Landscapes

  • Physics & Mathematics (AREA)
  • 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)
  • Treatment Of Fiber Materials (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention relates to a kind of lossless rapid detection methods of Xinjiang coloured silk cotton interior quality near infrared spectrum, this method is by the foundation of the measure of sample parameters value, sample sets classification, sample near infrared spectrum scanning and sample sets, editor's brown coloured silk cotton each sample collection, establishes quantitative calibration models, optimization quantitative calibration models and the completion of quick detecting step, pass through computerized near infrared scan cotton fiber, the spectrum based on content of material is obtained, feasible means are provided for characterization fiber quality.It solves the key technology difficulty that color cotton runs into terms of purchasing with quality identification in processing link at present, is worth promoting and applying in color cotton quality identification.

Description

The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum
Technical field
The present invention relates to a kind of lossless rapid detection methods of Xinjiang coloured silk cotton interior quality near infrared spectrum.
Background technology
Xinjiang is carried out in the leading position in color cotton research and development field, many color cotton research institutions in Xinjiang and enterprise A large amount of fruitful work such as conventional breeding, molecular mark, transgenic breeding, end 2012 years, Xinjiang is common Color cotton new varieties 23 are authorized, the fiber quality of new varieties is all significantly improved.But colorful cotton fibre quality-improving according to It is so the hot and difficult issue problem in current color cotton breeding work.
Because fiber quality is the quantitative character of controlled by multiple genes, quality can not intuitively embody, it is necessary to specific instrument Device;Expensive, the service requirement constant temperature and humidity currently used for color cotton fiber attribute test instrument, and, inspection low in my area's ownership It surveys costly;Therefore many breeders have to the quantity for significantly compressing species test material during the selection and breeding of field, Just it is present with leakage sieve during this, wastes hard-earned intermediate materials.Therefore there is an urgent need to one kind for Breeding of Color Cotton work Simply, fast, low cost detection fiber quality method, solve fiber quality detection common problem.
The problem of existing detection means is insufficient during colorful cotton fibre quality breeding and many are engaged in wheat, big The same problems that the researcher of the crop breedings such as beans, corn, watermelon work faces.
For limitation and deficiency existing for current color cotton fiber quality determination instrument, propose to utilize near infrared spectroscopy instrument The method that fast quantitative analysis is carried out at the same time to a variety of qualities of color cotton.It this method solve current Xinjiang coloured silk cotton Quality Detection side The problems such as tester is expensive existing for method, test laboratory environment requirement constant temperature and humidity, testing cost is high.
Near-infrared spectral analytical method is that the frequency multiplication of X-H groups (X=H, C, N, O) or sum of fundamental frequencies absorb in recorded matter, Qualitative and quantitative analysis can be carried out by the method processing of Chemical Measurement.Different from general analysis method, its application needs Quantitative or qualitative mathematics model is established in advance.
The flow of Near-Infrared Spectra for Quantitative Analysis is divided into two big steps:That is founding mathematical models (analysis method, prediction side Journey) and examine, the stability of Optimized model;And applied mathematical model, using the near infrared spectrum of unknown sample, prediction is not Know content or property in relation to component in sample.
The near infrared spectrum of measured matter depends on the Nomenclature Composition and Structure of Complexes of sample in near-infrared spectrum analysis.The group of sample Into there is certain functional relation between structure and near infrared spectrum.Determine that these are important using chemometrics method Functional relation, i.e., it is corrected, it is possible to according to the near infrared spectrum of sample, quickly to calculate the content of various components. Near-infrared spectral analytical method has compared with other analysis methods:Analyze speed is fast, and measurement process mostly can be complete in 1min Into;Analysis efficiency is high, can be simultaneously to multiple components of sample by a spectral measurement and established corresponding calibration model Or property is measured, and provides qualitative, quantitative result;Applicable sample scope is wide, can be direct by corresponding test sample device The sample spectra measurement for measuring the different states of matters such as liquid, solid, semisolid and colloid is convenient;Sample need not generally be located in advance Reason, need not use the test conditions such as chemical reagent or high temperature, high pressure, high current, will not be generated after analysis chemistry, biology or Electromagnetic pollution;Analysis cost it is relatively low (without numerous and diverse pretreatment, can multicomponent detect simultaneously, test favorable reproducibility;To sample without Damage does not influence the two time selling of sample;Requirement to operating personnel is not harsh, can be competent by simply training Etc. exclusive technical advantage, therefore near infrared spectrum, in food security, the fields such as food quality and Chinese herbal medicine quality identification obtain Extensive use is arrived.
Up to the present, the document using the lossless quick detection coloured silk cotton interior quality of nearly red spectral is had no, but in spectroscopy With finding one " cotton seed oil content near-infrared Nondestructive Detection model and application " on spectrum analysis magazine, the document is ground The object studied carefully is the cottonseed oil of land white cotton, and the content of land white cottonseed oil is carried out using near-infrared spectrum technique Lossless, quick detection.And the present invention relates to the brown color cotton fiber index of quality, the object domain and document of research are completely It is different.
Numerous researchs show:Colorful cotton fibre is mainly by cellulose, hemicellulose, cellulose accompaniment and coloring matter Composition, cellulose accompaniment grade including soluble saccharide, wax, fat, protein, pectic substance, chlorine-bearing compound and ash, remove Outside ash content, containing X-H groups (X=H, C, N, O) in other materials, this is just to predict this in fiber using near infrared spectrum The content of a little substances has established material base.
What is more important, by numerous studies, fiber quality is also closely related with the content of these substances.By near red Outer optical scanning cotton fiber, obtains the spectrum based on content of material, and feasible means are provided for characterization fiber quality.
Research shows that the qualitative character of crop and inherent content of predetermined substance are closely related, no matter watermelon, corn and soybean Or cotton considers that, all containing X-H groups (X=H, C, N, O), these groups can be reflected as from the most small structure of matter The difference of near infrared spectrum, therefore, Different Crop quality trait near-infrared assistant breeding for the angle of near infrared spectrum, With general character, can use for reference.
The content of the invention
Present invention aims at, provide a kind of Xinjiang coloured silk cotton interior quality near infrared spectrum lossless rapid detection method, it should Method be classified by the measure of sample parameters value, sample sets, foundation, the editor palm fibre of sample near infrared spectrum scanning and sample sets Color cotton each sample collection establishes quantitative calibration models, optimization quantitative calibration models and the completion of quick detecting step, by near red Outer optical scanning cotton fiber, obtains the spectrum based on content of material, and feasible means are provided for characterization fiber quality.Solution Determined current color cotton purchase and processing link in the key technology difficulty that runs into terms of quality identification, be worth in color cotton quality It is promoted and applied in identification.
A kind of lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum of the present invention, follows these steps It carries out:
A, the measure of sample parameters value:The brown coloured silk cotton that impurity removing is cleaned out, is numbered, with fibrometer system point The other interior quality long to mic value, intensity, elongation and the upper half of each brown cotton sample product is analyzed, and obtains palm fibre The detection data of color cotton interior quality, i.e. quality determination value;
B, sample sets are classified:The sample of the brown coloured silk cotton interior quality measured value obtained in step a is divided into correcting sample Collection, verification sample collection and Prediction, Calibration and verification sample collection are used for establishing quantitative calibration models, pre- test sample Product collection is used for evaluating the accuracy and validity of the model, and wherein Calibration accounts for the 60% of sample total amount, verification sample collection For 20%, Prediction 20%;
C, the foundation of sample near infrared spectrum scanning and sample sets:Step b is obtained respectively near infrared spectroscopy instrument Calibration, verification sample collection and the Prediction of brown coloured silk cotton carry out near infrared spectrum scanning, respectively obtain brown coloured silk Cotton sample product Calibration, verification sample collection and Prediction near infrared spectrum scanning figure;
D, brown coloured silk cotton each sample collection is edited:By the sample sets obtained in step c since Calibration, by all schools The collection of illustrative plates of positive sample sets infrared diaphanoscopy according to Calibration serial number order, is imported near infrared spectrometer in batches " model and sample sets management " section, establishes brown cotton Calibration in this section, and to the Calibration into edlin: Calibration is opened, the mic value of brown coloured silk cotton sample product, intensity, elongation in step a are added on Calibration section The title and its corresponding quality determination value of rate and the long interior quality of upper half, the correcting sample editted are concentrated, each sample Include atlas of near infrared spectra and corresponding four kinds of quality determination values;
It establishes brown coloured silk cotton verification sample collection and Prediction is carried out as the step of Calibration, by all samples After collection establishes, in " sample sets management " section, it is seen that established brown coloured silk cotton Calibration, verification sample collection and pre- Sample collection;
E, quantitative calibration models are established:In near infrared spectrometer " model management " section, by established correction in step d Sample sets and verification sample collection are imported into model foundation software, with Partial Least Squares Regression quantitative approach, selection 1100nm-2400nm bands are modeling wave band, and under the conditions of the modeling parameters of system default and Pretreated spectra, it is fixed to establish Measure calibration model, modeling software using import and the modeling configuration condition of selection under calculate quantitative calibration models automatically, and give Go out the prediction result figure of quantitative calibration models and corresponding model parameter, four kinds of brown coloured silk cotton is obtained in " model management " section The quantitative calibration models of quality;
F, quantitative calibration models are optimized:Using modeling software editting function, to the four kinds of product of brown coloured silk cotton obtained in step e Matter quantitative calibration models are modified and are optimized, and model optimization process is:Only change modeling wave band every time, other modeling configurations It is remained unchanged with Pretreated spectra mode, establishes the quantitative calibration models of different-waveband, quantified by comparing each modeling wave band The evaluating of calibration model:Calibration set standard deviation, cross-verification collection standard deviation and forecast set standard deviation and reference are quantitative Calibration model calibration set predicted value and measured value related coefficient, select calibration set standard deviation, K=fold cross-verification collection standards Difference and forecast set standard deviation are minimum, the modeling ripple of quantitative calibration models calibration set predicted value and measured value related coefficient maximum Two bands of section 1300nm-1700nm and 1800nm-2400nm model wave band for four kinds of qualities of brown coloured silk cotton;Then select It is constant to select best modeled wave band, only changes Pretreated spectra mode, establishes the quantitative correction mould under different Pretreated spectra modes Type, it is similary to select calibration set standard deviation by comparing the evaluating of quantitative calibration models under each Pretreated spectra mode, Cross-verification collection standard deviation and forecast set standard deviation are minimum, quantitative calibration models calibration set predicted value and measured value related coefficient Maximum Savitzky-Golay is smooth, and Savitzky-Golay derivative spectrums pretreatment mode is four kinds of qualities of brown coloured silk cotton Pretreated spectra mode is modeled, finally with two region modeling wave bands of 1300nm-1700nm and 1800nm-2400nm and light Savitzky-Golay is smooth, and Savitzky-Golay derivatives spectrum pretreatment mode establishes quantitative calibration models, which is Four kinds of quantitative calibration models best in quality of brown coloured silk cotton;
G, brown coloured silk cotton Prediction 0.1g-1.5g in step b is placed near infrared spectrometer sample preheated in advance In product disk, through near infrared spectrum scanning, the optimal quantitative calibration models that are obtained in steps for importing f are to get to brown coloured silk cotton sample product The prediction result of corresponding interior quality.
The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum of the present invention, brown is color in this method Cotton interior quality index:
Upper half is long:Brown coloured silk cotton upper half mean length upper-half-mean length brown color cotton fiber length During measure, weight accounts for the average length of the radical of the longer fibers part of fibre bundle half (50%), and it is equal to be commonly abbreviated as upper half Long, unit is millimeter;
Mic value:The a certain amount of brown color cotton fibers of mic value micronaire value under prescribed conditions ventilative The measurement of property, is the overall target of cotton fiber fineness and maturity and determines that this index does not have unit.
Regularity:Uniformity index uniformity index, during brown color cotton fiber length measurment, average length with it is upper The ratio between half portion average length represents that unit is represented with percentage (%) with the percentage of upper half mean length.
Elongation:Length when color cotton fiber is stretched to straight line, unit are represented with (%).
These four above-mentioned indexs are that must examine to refer in the most important index of quality of color cotton and color cotton quality grading inspection Mark is purchased in color cotton, and processing and color cotton breeding field will carry out color cotton fiber quality according to the measured value of these indexs Classification.Therefore a kind of simple and direct, quick, colleges and universities are established, be suitble to the quantitative detecting method of the high-volume index of quality color cotton breeding, Purchase and manufacture field have Great significance.
The quality parameter value of color cotton sample product (brown coloured silk cotton) be with USTER fibrometer systems the laboratory of constant temperature and humidity into What row measured, all coloured silk cotton sample product and its quality parameter measured value are provided by Xinjiang Cai Mian research institutes.Brown coloured silk cotton sample number It measures as 7356.
Description of the drawings
Fig. 1 is the original atlas of near infrared spectra of brown coloured silk cotton calibration set of the present invention;
Fig. 2 is the optimal main cause subnumber distribution map of the long quantitative calibration models of brown coloured silk cotton upper half of the present invention;
Fig. 3 for PLS calibration models of the present invention to the long prediction result figure of brown cotton upper half, wherein-О-correcting sample Collection ,-Δ-verification sample collection;
Fig. 4 is the optimal main cause subnumber distribution map of brown coloured silk cotton mic value quantitative calibration models of the present invention;
Fig. 5 for PLS calibration models of the present invention to brown cotton mic value prediction result figure, wherein-О-correcting sample Collection ,-Δ-verification sample collection;
Fig. 6 is the optimal main cause subnumber distribution map of brown coloured silk cotton elongation quantitative calibration models of the present invention;
Fig. 7 is the prediction result figure that PLS calibration models of the present invention extend brown cotton, wherein-О-Calibration ,- Δ-verification sample collection;
Fig. 8 is the optimal main cause subnumber distribution map of brown coloured silk cotton regularity quantitative calibration models of the present invention;
Fig. 9 is prediction result figure of the PLS calibration models of the present invention to brown cotton regularity, wherein-О-correcting sample Collection ,-Δ-verification sample collection.
Specific embodiment
Embodiment
The measure of sample parameters value:The brown coloured silk cotton sample product that impurity removing is cleaned out, each weigh 0.1g-1.5g, into Row number, with fibrometer system respectively in mic value, intensity, elongation and the upper half length of each brown cotton sample product It is analyzed in the index of quality, obtains the detection data i.e. product of the long interior quality of mic value, intensity, elongation and upper half Matter index determining value;
Sample sets are classified:The interior quality measured value sample obtained in step a is divided into Calibration, verification sample collection And Prediction, Calibration and verification sample collection are used for establishing quantitative calibration models, Prediction is used for evaluating this The accuracy and validity of model, wherein Calibration account for the 60% of sample total amount, and verification sample collection is 20%, pre- test sample Product collection is 20%;Brown coloured silk cotton Calibration, verification sample concentrate the distribution situation distribution of each index of quality measured value to be shown in Table 1:
1 brown coloured silk cotton calibration set of table and verification collect the distribution of each quality content
The foundation of sample near infrared spectrum scanning and sample sets:It (is produced near infrared spectroscopy instrument in Chinese optically focused science and technology Near infrared spectrometer SUPNIR 2700) respectively to the Calibration of the obtained brown coloured silk cottons of step b, verification sample collection and pre- Sample collection carries out near infrared spectrum scanning, takes brown coloured silk cotton sample product 0.1g-1.5g every time, is placed in the rotation of near infrared spectrum In diffusing reflection sampler tray, using background built in instrument as reference, with Rotating with Uniform pattern, color cotton sample product near infrared spectrum is gathered, often Twice, sweep parameter is set a Sample Scan:Spectra collection scope 1000nm-2400nm, scanning times 32 times, resolution ratio 8cm- 1, a data point is gathered per 4cm, gathers 1500 data altogether, scans 22 DEG C of temperature, brown coloured silk cotton Calibration and verification For sample sets infrared spectrum stacking chart as shown in Figure 1, abscissa is wavelength (nm), ordinate is absorbance (A);
Edit brown coloured silk cotton each sample collection:Since calibration set, the collection of illustrative plates of all calibration set sample infrared diaphanoscopies is pressed According to Calibration serial number order, " model and sample sets management " section is imported near infrared spectrometer in batches, in this section Brown cotton Calibration is established in face, and to the Calibration into edlin:Calibration is opened, is cut in Calibration The long interior quality of mic value, intensity, elongation and upper half of brown cotton sample product and its corresponding product in step a are added on face Matter measured value, the correcting sample editted are concentrated, and each sample should include atlas of near infrared spectra and corresponding quality determination value; It establishes brown coloured silk cotton verification sample collection and Prediction is carried out as the step of Calibration, cut in " sample sets management " See brown cotton Calibration, verification sample collection and Prediction in face;
Establish quantitative calibration models:The RIMP.P003.V01B.001 softwares carried using near infrared spectrometer, from brown In the near infrared spectrum scanning collection of illustrative plates of color cotton Calibration it can be seen that, it is evident that characteristic absorption peak:Exist respectively At 1300nm-1670nm and at 1870-2220nm and at 2220nm-2430nm, chemometrics method-minimum two is utilized Multiply recurrence computational methods, by these near infrared spectrum characteristic absorption peak datas of brown coloured silk cotton and its interior quality mic value, on Partly long, intensity establishes corresponding relation between elongation, in the Pretreated spectra side of near infrared spectrometer modeling software acquiescence Method and selection selection all band, extract the information of efficient association between color cotton interior quality and its near-infrared absorption spectrum, establish The quantitative calibration models of corresponding quality parameter;
Optimize quantitative calibration models:In color cotton near infrared spectrum containing random noise, baseline drift, sample be uneven, light Interference caused by the factors such as scattering can eliminate various noises and interference with rational Pretreated spectra means, and it is near to extract color cotton The characteristic information of infrared spectrum improves the stability and precision of prediction of calibration model, utilizes the light for changing near infrared spectrum and carrying Preprocess method modeling parameters are composed, edit-modify are carried out to the quantitative calibration models built up respectively, according to fixed in editing process Measure the calibration set standard deviation (SEC) of calibration model, K=fold cross-verification collection standard deviations (SECV) and verification collection standard deviation (SEP) size of value and degree close to each other continuously edit calibration model, wherein the calibration set standard of calibration model Poor (SEC), K=fold cross-verification collection standard deviations (SECV) and verification collection standard deviation (SEP) value smaller (closer to zero) and It is closer better between each other simultaneously, when calibration set predicted value and measured value related coefficient (RC) closer 1, the school established The prediction effect of positive model is preferable, according to mentioned above principle, only changes modeling wave band every time, other modeling configurations are located in advance with spectrum Reason mode remains unchanged, and establishes the quantitative calibration models of different-waveband, by comparing each modeling wave band quantitative calibration models Evaluating:Calibration set standard deviation, cross-verification collection standard deviation and forecast set standard deviation and reference quantitative calibration models school Positive collection predicted value and measured value related coefficient, select calibration set standard deviation, cross-verification collection standard deviation and forecast set standard deviation Minimum, the modeling wave band 1300nm-1700nm of quantitative calibration models calibration set predicted value and measured value related coefficient maximum and Two bands of 1800nm-2400nm model wave band for four kinds of qualities of brown coloured silk cotton;Then best modeled wave band is selected not Become, only change Pretreated spectra mode, establish the quantitative calibration models under different Pretreated spectra modes, it is each by comparing The evaluating of quantitative calibration models under Pretreated spectra mode, it is similary to select calibration set standard deviation, cross-verification collection standard deviation It is minimum with forecast set standard deviation, the Savitzky- of quantitative calibration models calibration set predicted value and measured value related coefficient maximum Golay is smooth, and Savitzky-Golay derivative spectrums pretreatment mode models Pretreated spectra side for four kinds of qualities of brown coloured silk cotton Formula, it is finally smooth with two region modeling wave bands of 1300nm-1700nm and 1800nm-2400nm and light Savitzky-Golay, Savitzky-Golay derivatives compose pretreatment mode, establish quantitative calibration models, and the model is best in quality for four kinds of brown coloured silk cotton Quantitative calibration models;The method screening that a kind of fixed pretreatment item and other pretreatment items are respectively combined every time is most preferably located in advance Reason method by being tested with processing method combined sorting, finally determines that Savitzky-Golay is smooth, Savitzky-Golay Derivative, both preprocess methods are combined as the final preprocess method of interior quality calibration model in color cotton four;Finally use At 1300nm-1700nm and at 1800-2400nm, two bands and Savitzky-Golay are smooth, Savitzky- Golay derivative spectrum preprocess methods establish the quantitative calibration models of brown coloured silk four kinds of qualities of cotton, which is total four kinds of color The optimal quantitative calibration models of the index of quality;
Principle is evaluated using calibration model, respectively to four kinds of crucial interior qualities of brown coloured silk cotton:Mic value, intensity are stretched It is equal that long rate and the long quantitative calibration models progress of upper half respectively obtain mic value, intensity, elongation and upper half after further optimizing The optimal quantitative calibration models of long brown coloured silk cotton interior quality index, brown coloured silk cotton mic value, intensity, elongation and upper half The sum of the prediction result figure of long interior quality quantitative calibration models and cross-verification square-error (PRESS) figure, are shown in Fig. 2-figure 9, wherein Fig. 2, Fig. 4, Fig. 6, Fig. 8 is (PRESS) figure, is the selection gist of quantitative calibration models main cause subnumber, minimum in figure The corresponding main cause subnumber of PRESS values is the optimal main cause subnumber of quantitative calibration models;Fig. 3, Fig. 5, Fig. 7, Fig. 9 are brown coloured silk cotton The prediction result figure of quality quantitative calibration models in four;
From Fig. 3, Fig. 5, Fig. 7, Fig. 9, brown coloured silk cotton upper half length, mic value, elongation, in regularity four There are linear relationship between the predicted value and measured value of the near-infrared quantitative calibration models of the index of quality, quantitative model is corrected Calibration set standard deviation (SEC), verification collection standard deviation (SEP), K=fold cross-verification collection standard deviation (SECV) value is smaller, together When the mutual gap of these parameter values it is also smaller, three parameter values are relatively close together, and accord with K=fold cross-verification collection standard deviations (SECV), verification collection standard deviation (SEP) value >=SEC*1.5, the measured value related coefficient (RC) of four kinds of interior quality calibration models Value is all higher than 0.92, illustrates that these four interior quality calibration models of brown coloured silk cotton have preferably predictive ability, what model obtained Correlation between predicted value and measured value is very good, brown coloured silk cotton sample product near infrared spectrum and brown coloured silk cotton interior quality it Between there are linear correlation, reached preferable prediction result, show this method in four kinds of quantitative analysis brown coloured silk cotton in product Matter index is feasible;
The long interior quality quantitative correction mould of brown coloured silk cotton mic value, intensity, elongation and upper half that the present invention establishes Type estimated performance evaluation result is shown in Table 2:
2 brown coloured silk cotton PLS quantitative calibration models estimated performance evaluation results of table
Brown coloured silk cotton mic value, intensity, elongation and the long interior quality ginseng near-infrared quantitative calibration models SEP of upper half It disclosure satisfy that the quantitative analysis error requirements of color cotton quality, the quantitative calibration models of foundation are applied to Xinjiang brown coloured silk cotton mark In grand value, intensity, elongation and long the quick of interior quality of upper half, nondestruction quantitative analysis;
Evaluation to the estimated performance of model:It is optimal to import brown coloured silk cotton for the model evaluation software carried using instrument Quantitative calibration models, the Prediction editted, near infrared spectrometer analysis system software will just provide less than one minute The prediction result of quality and predicted value (are detected with measured value with Wu Site fibrometer systems in the four of all forecast sets imported Obtained measured value) between absolute deviation;Quantitative calibration models are to brown coloured silk cotton mic value, intensity, elongation and upper half The prediction result of these four interior qualities is grown respectively at the survey measured with four kinds of interior qualities with Wu Site fibrometer systems Definite value is compared, and statistical result is listed in table 3- tables 6 respectively:
The long calibration model prediction result of the brown cotton upper half of table 3
The brown cotton mic value calibration model prediction result of table 4
The brown cotton elongation calibration model prediction result of table 5
6 brown cotton regularity calibration model prediction results
It can be seen that by the data of table 3- tables 6:Color cotton mic value, intensity, elongation and upper half grow four kinds of interior qualities Index corrects quantitative model predicted value with it with compared with large capacity Wu Site fibrometer system measured values with near-infrared, these The prediction error of index illustrates to utilize established near-infrared in the range of the admissible analytical error of these index of quality Quantitative model is corrected, it is feasible to carry out quick nondestructive quantitative analysis to color four kinds of interior qualities of cotton.
Conclusion
Nothing is carried out to color cotton mic value, intensity, elongation and the long interior quality of upper half using near-infrared spectrum technique Damage rapid detection method with the fibrometer system detection method applied at present compared with have it is easy to operate, it is at low cost (staff training with Instrument and environment and energy consumption etc.), speed is fast, efficient, not harsh to experimental situation requirement, is particularly suitable for the color cotton sample of high-volume The Rapid identification of product, must be permanent unlike fibrometer system to experimental situation requirement because near infrared spectroscopy instrument is small Near infrared spectroscopy instrument is taken in actual cotton purchase and manufacture field, can solved in these fields by the condition of constant temperature and humidity The superiority that can not be realized using fibrometer system device at present.Color cotton fiber Quality Detection classification aspect has been well solved to exist The technical barrier that purchase and manufacture field are run into.At present because the requirement of fibrometer system device experimental situation is high, in purchase link Partly long, the indexs such as elongation still pull tape measurement with hand, and sample measures testing staff one by one, during this also Estimate and test, regularity, other indexs such as mic value.This method need to pass through certain professional skill to the more demanding of operating personnel The personnel of training can implement this work.Hand pulls the usual checkout procedure of tape measurement and takes longer, and labor intensive is larger, can not Meet the requirement that bag is examined.
The method of the invention solves the key that color cotton runs into terms of purchasing with quality identification in processing link at present Technical barrier is worth promoting and applying in color cotton quality identification.

Claims (1)

1. a kind of lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum, it is characterised in that follow these steps into Row:
A, the measure of sample parameters value:The brown coloured silk cotton that impurity removing is cleaned out, is numbered, right respectively with fibrometer system The interior quality that mic value, intensity, elongation and the upper half of each brown coloured silk cotton sample product are long is analyzed, and obtains brown The detection data of color cotton interior quality, i.e. quality determination value;
B, sample sets are classified:The sample of the brown coloured silk cotton interior quality measured value obtained in step a is divided into Calibration, is tested Sample sets and Prediction are demonstrate,proved, Calibration and verification sample collection are used for establishing quantitative calibration models, and Prediction is used Evaluate the accuracy of the model and validity, wherein Calibration accounts for the 60% of sample total amount, verification sample collection is 20%, in advance Sample collection is 20%;
C, the foundation of sample near infrared spectrum scanning and sample sets:The brown obtained respectively to step b near infrared spectroscopy instrument Calibration, verification sample collection and the Prediction of color cotton carry out near infrared spectrum scanning, respectively obtain brown coloured silk cotton sample Product Calibration, verification sample collection and Prediction near infrared spectrum scanning figure;
D, brown coloured silk cotton each sample collection is edited:By the sample sets obtained in step c since Calibration, by all correction samples The collection of illustrative plates of product collection infrared diaphanoscopy, according to Calibration serial number order, imported into batches near infrared spectrometer " model and Sample sets management " section, establishes brown coloured silk cotton Calibration in this section, and to the Calibration into edlin:It opens Calibration, added on Calibration section the mic value of brown coloured silk cotton sample product in step a, intensity, elongation and The title and its corresponding quality determination value of the long interior quality of upper half, the correcting sample editted are concentrated, and each sample includes Atlas of near infrared spectra and corresponding four kinds of quality determination values;
It establishes brown coloured silk cotton verification sample collection and Prediction is carried out as the step of Calibration, all samples collection is built After standing well, in " sample sets management " section, it is seen that established brown coloured silk cotton Calibration, verification sample collection and pre- sample Collection;
E, quantitative calibration models are established:In near infrared spectrometer " model management " section, by established correcting sample in step d Collection and verification sample collection are imported into model foundation software, with Partial Least Squares Regression quantitative approach, select 1300nm- 1700nm is modeling wave band with two bands of 1800nm-2400nm, in the modeling parameters and Pretreated spectra of system default Under the conditions of, quantitative calibration models are established, modeling software is quantitative using being calculated automatically under the modeling configuration condition for importing and selecting Calibration model, and the prediction result figure of quantitative calibration model and corresponding model parameter, obtain in " model management " section The quantitative calibration models of brown coloured silk four kinds of qualities of cotton;
F, quantitative calibration models are optimized:Using modeling software editting function, the four kinds of qualities of brown coloured silk cotton obtained in step e are determined Amount calibration model is modified and is optimized, and model optimization process is:Only change modeling wave band every time, other modeling configurations and spectrum Pretreatment mode remains unchanged, and establishes the quantitative calibration models of different-waveband, by comparing each modeling wave band quantitative correction mould The evaluating of type:Calibration set standard deviation, cross-verification collection standard deviation and forecast set standard deviation and reference quantitative correction mould Type calibration set predicted value and measured value related coefficient, select calibration set standard deviation, cross-verification collection standard deviation and forecast set standard Difference is minimum, the modeling wave band 1300nm-1700nm of quantitative calibration models calibration set predicted value and measured value related coefficient maximum With 1800nm-2400nm wave band is modeled for four kinds of qualities of brown coloured silk cotton;Then select this two modeling wave bands constant, only change light Pretreatment mode is composed, the quantitative calibration models under different Pretreated spectra modes are established, by comparing each Pretreated spectra side The evaluating of quantitative calibration models under formula, it is similary to select calibration set standard deviation, cross-verification collection standard deviation and forecast set standard Poor minimum, quantitative calibration models calibration set predicted value and the Pretreated spectra mode of measured value related coefficient related coefficient maximum are The optimal spectrum pretreatment mode of four kinds of qualities of brown coloured silk cotton finally selects 1300nm-1700nm and 1800nm-2400nm to model Wave band and Savitzky-Golay are smooth, and Savitzky-Golay derivative spectrum pretreatment modes establish quantitative calibration models, should Model is four kinds of quantitative calibration models best in quality of brown coloured silk cotton;
G, brown coloured silk cotton Prediction 0.1g-1.5g in step b is placed near infrared spectrometer sample disc preheated in advance In, through near infrared spectrum scanning, the optimal quantitative calibration models obtained in steps for importing f are answered to get to brown coloured silk cotton sample condition The prediction result of interior quality.
CN201711267876.2A 2017-12-05 2017-12-05 The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum Pending CN108061724A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711267876.2A CN108061724A (en) 2017-12-05 2017-12-05 The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711267876.2A CN108061724A (en) 2017-12-05 2017-12-05 The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum

Publications (1)

Publication Number Publication Date
CN108061724A true CN108061724A (en) 2018-05-22

Family

ID=62136205

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711267876.2A Pending CN108061724A (en) 2017-12-05 2017-12-05 The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum

Country Status (1)

Country Link
CN (1) CN108061724A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112098357A (en) * 2020-08-21 2020-12-18 南京农业大学 Strawberry sensory quality grade evaluation method based on near infrared spectrum
CN112649391A (en) * 2020-12-03 2021-04-13 浙江大学 Fiber quality grade online detection system and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
JOSEPH G. MONTALVO等: "Studies to measure cotton fibre length,strength, micronaire and colour by vis/NIRreflectance spectroscopy.Part II: Principal components regression", 《NEAR INFRARED SPECTROSC》 *
YONGLIANG LIU等: "Application of near infrared spectroscopy in cotton", 《INFORMATION PROCESSING IN AGRICULTURE》 *
孙武勇等: "近红外光谱技术在棉纤维品质检测和产地溯源中的研究进展", 《中国农学通报》 *
江苏: "近红外技术在烟用辅料质量控制中的应用研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112098357A (en) * 2020-08-21 2020-12-18 南京农业大学 Strawberry sensory quality grade evaluation method based on near infrared spectrum
CN112098357B (en) * 2020-08-21 2021-12-10 南京农业大学 Strawberry sensory quality grade evaluation method based on near infrared spectrum
CN112649391A (en) * 2020-12-03 2021-04-13 浙江大学 Fiber quality grade online detection system and application thereof

Similar Documents

Publication Publication Date Title
CN100590417C (en) Plant blade physiologic index non-destructive test method
CN101308086B (en) Fruit internal quality on-line checking apparatus based on near infrared spectra technology
CN101769866B (en) Device for detecting milk components and method thereof
CN102879353B (en) The method of content of protein components near infrared detection peanut
CN103645155B (en) The fast non-destructive detection method of fresh mutton tenderness
CN101413885A (en) Near-infrared spectrum method for rapidly quantifying honey quality
JPH03504769A (en) Method and apparatus for spectroscopic comparison of compositions
CN104390927B (en) The quick determination method of ash content in coal sample
CN107091815A (en) A kind of method for identifying rosewood
CN105548062B (en) The quick nondestructive synchronization detecting method of fresh beef appetizer multi objective
CN109211829A (en) A method of moisture content in the near infrared spectroscopy measurement rice based on SiPLS
CN106950192A (en) A kind of method of Contents of Main Components quick detection in vegetable protein beverage based on near-infrared spectral analysis technology
CN107860743A (en) Utilize the method and its application of the model of reflective near infrared fibre-optical probe structure fast prediction oil property
CN108061724A (en) The lossless rapid detection method of Xinjiang coloured silk cotton interior quality near infrared spectrum
CN108827907A (en) It is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration
CN104849234A (en) Assay method for analyzing contents of principal components of imidacloprid based on near-infrared spectrum
CN108169168A (en) Test and analyze rice grain protein content mathematical model and construction method and application
CN109100315B (en) Wavelength selection method based on noise-signal ratio
CN110231306A (en) A kind of method of lossless, the quick odd sub- seed protein content of measurement
CN110231302A (en) A kind of method of the odd sub- seed crude fat content of quick measurement
CN102519903B (en) Method for measuring whiteness value of Agaricus bisporus by using near infrared spectrum
CN106198423B (en) A method of ham sausage grade is identified based on visible-near-infrared spectrum analytical technology
CN110057756A (en) A kind of infrared photoacoustic spectra detection method of wheat flour quality
CN106053380A (en) Method for quickly analyzing proportions of tree species of mixed pulp wood by aid of near infrared spectrum technologies
CN101387497A (en) Method for measuring plant fiber material fibre morphology by near-infrared spectrum technology

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination