CN110646324A - Method for measuring relative density of tobacco essence and flavor - Google Patents
Method for measuring relative density of tobacco essence and flavor Download PDFInfo
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- 239000000796 flavoring agent Substances 0.000 title claims abstract description 57
- 235000019634 flavors Nutrition 0.000 title claims abstract description 57
- 241000208125 Nicotiana Species 0.000 title claims abstract description 53
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000011159 matrix material Substances 0.000 claims abstract description 207
- 238000001228 spectrum Methods 0.000 claims abstract description 48
- 239000003205 fragrance Substances 0.000 claims abstract description 45
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 7
- 230000003595 spectral effect Effects 0.000 claims description 67
- 235000013599 spices Nutrition 0.000 claims description 26
- 238000012360 testing method Methods 0.000 claims description 25
- 239000002304 perfume Substances 0.000 claims description 14
- 235000019504 cigarettes Nutrition 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 238000001069 Raman spectroscopy Methods 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000001237 Raman spectrum Methods 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 238000010606 normalization Methods 0.000 claims description 3
- 238000005102 attenuated total reflection Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000013178 mathematical model Methods 0.000 abstract description 3
- 238000004566 IR spectroscopy Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 29
- 238000005259 measurement Methods 0.000 description 9
- 238000012937 correction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 238000007430 reference method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940116024 aftera Drugs 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002790 cross-validation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004476 mid-IR spectroscopy Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/24—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by observing the transmission of wave or particle radiation through the material
-
- 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
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- 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
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
-
- 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
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
The invention discloses a relative density determination method of tobacco flavor and fragrance, which comprises the steps of obtaining an infrared spectrogram of the tobacco flavor and fragrance and a relative density value of the tobacco flavor and fragrance to obtain a spectrum matrix and a numerical matrix of a flavor and fragrance sample, establishing a relative density model of the tobacco flavor and fragrance based on a partial least square method, obtaining a spectrum matrix component and a numerical matrix component of which the spectrum matrix and the numerical matrix conform to the maximum variance by the partial least square method, establishing a corresponding mathematical model of the relative density value of the tobacco flavor and fragrance and a near-infrared spectrogram according to all the obtained spectrum matrix component and numerical matrix component, and obtaining the relative density value of the flavor and fragrance by obtaining the infrared spectrum numerical value doctor mathematical model of the flavor and fragrance which needs to measure the relative density, wherein the method is simple, the infrared spectrogram of the tobacco flavor and fragrance can be accurately obtained by the infrared spectroscopy, the detection precision is high, and the determination of the relative density content of the tobacco flavor and fragrance can be rapidly and accurately realized.
Description
Technical Field
The invention relates to the technical field of tobacco, in particular to a method for measuring relative density of tobacco flavor and fragrance.
Background
The tobacco essence perfume has the functions of improving the smoking quality of cigarettes and endowing the cigarettes with characteristic fragrance, and is an important factor forming the brand style of the cigarettes. Whether the quality of different batches of essence and spice products is stable or not is closely related to the quality stability of cigarette products. However, the complexity and diversity of chemical components of the formed flavors and fragrances are always the key and difficult points of quality control due to the influence of various factors such as raw materials and processing. Therefore, it is necessary to perform a comprehensive evaluation on the quality of the flavor for tobacco, wherein the physical indexes for evaluating whether the quality of the flavor is stable include relative density and refractive index. The existing method for measuring relative density adopts a chemical method, when a plurality of essence and spice samples with different brands are continuously detected in batches, instruments after each sample is measured are cleaned and dried, and the influence on the accurate and quick completion of the measurement work is large. If the instrument is not cleaned after each measurement, the residual sample in the previous measurement interferes with the next measurement, and the accuracy of the measurement result is influenced; if the instrument is set to wash and dry too long, the measurement time is extended and the reagents for analysis are wasted. Therefore, when the essence and flavor for cigarettes of different brands are continuously measured in a large scale, the technical problem that the measurement result is inaccurate or the measurement efficiency is low can occur, and the technical problem needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for measuring the relative density of tobacco flavor and fragrance, which overcomes the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring relative density of tobacco essence and flavor comprises the following steps:
step 1), obtaining a spectrogram of a flavor and fragrance sample, and obtaining a spectral matrix E of the flavor and fragrance sample according to the obtained spectrogram;
step 2), obtaining the relative density value of the essence and spice sample, and establishing a relative density numerical matrix F of the essence and spice sample according to the relative density value of the essence and spice sample;
step 3), establishing a relative density model of the tobacco essence perfume based on a partial least square method:
standardizing the spectrum matrix E to obtain the standardized spectrum matrix EiNormalizing the relative density numerical matrix F to obtain a normalized relative density numerical matrix FiIn the spectral matrix EiExtracting the spectral matrix component tiIn a matrix of relative density values FiExtracting relative density numerical value matrix component uiMaking the acquired spectral matrix component tiAnd relative density numerical matrix component uiThe maximum variance is met, i.e.:
Cov(ti,ui)–>max；
cov is the covariance sign, max is the maximum sign;
establishing spectral matrix components tiAnd relative density numerical matrix component uiMaximum variance expression of (2):
max<EiWi+1,FiCi+1>；
Wi+1is a spectral weight coefficient, Ci+1Is a numerical weight coefficient;
obtaining W through Lagrange solutioni+1And Ci+1Value, where Wi+1||＝1；||Ci+1||＝1,i≥0；
According to Wi+1And Ci+1The spectrum matrix component t with the maximum variance is obtained by inverse solutioniAnd relative density numerical matrix component ui；
According to the obtained spectral matrix component tiEstablishing a spectral matrix EiSpectral residual matrix E ofi-1For the spectral matrix component tiAccording to the component u of the matrix of the relative density valuesiEstablishing a relative density numerical matrix FiNumerical residual matrix F ofi-1For relative density numerical matrix component uiThe regression equation of (a):
Ei-1＝ti×p’i+Ei
Fi-1＝ui×q’i+Fi
Fi-1＝ti×r’i+Fi
wherein:
in the formula, piIs a spectral matrix EiOf the ith load vector, qiIs a relative density numerical matrix FiOf the ith load vector, riIs tiAnd uiThe relationship vector of (1);
obtaining a spectrum residual error matrix E according to the abovei-1Sum value residual error matrix Fi-1Obtaining a spectral matrix component ti-nRelative density matrix component ui-nSpectrum residual matrix Ei-nSum value residual error matrix Fi-n，nThe relative density main component quantity;
according to the acquired spectral matrix component ti-nAnd relative density numerical matrix component ui-nEstablishing a spectral matrix EiAnd relative density numerical matrix FiThe regression expression of (1):
Ei＝tip’i+ti-1p’i-1+...+tAp’A
Fi＝tir’i+ti-1r’i-1+...+tAr’A+FA
a is a spectral matrix EiAnd a matrix of relative density values FiThe rank of (d); t is t1,…,tARepresents E1，E2，…，EAThe linear combination of (a) and (b),
obtaining the expression of relative density:
in the formula, y*Is a relative density value, F(i-n)kAs a numerical residual matrix Fi-nThe kth line of (1); wherein { ak1,ak2,...,akmThe values of the regression coefficients are obtained; x is the number of1，x2，…，xmThe infrared spectrum data value of the essence and spice to be detected is obtained; and substituting the infrared spectrum data value of the essence and spice to be detected into the relative density expression to obtain the relative density value of the essence and spice to be detected.
Further, in the step 1), the essence and spice sample is dropped on an optical bench for infrared test or Raman test, so as to obtain an infrared spectrogram or Raman spectrogram of the essence and spice for the cigarette.
Further, the parameters of the spectrometer adopting the near infrared test are as follows: the scanning times are 4-256 times, and the resolution is 4cm-1～64cm-1Wavelength range of 10000cm-1～4000cm-1。
Further, the parameters of the spectrometer for performing the mid-infrared test are as follows: the scanning times are 2-256 times, and the resolution is 1cm-1～64cm-1Wavelength range 4000cm-1～400cm-1The spectrometer parameters for raman testing were: the scanning times are 2-64 times, the integration time is 500-5000 ms, and the wavelengthThe range is 152cm-1～2488cm-1。
Furthermore, the collection mode of the spectrogram comprises transmission, diffuse reflection and diffuse transflection.
Further, in the step 2), a gas chromatograph is adopted to measure the relative density value of the tobacco flavor and fragrance.
Further, in step 3), data standardization processing is performed on the spectral matrix E to obtain a standardized spectral matrix Ei(n × m), n is the number of samples, and m is the dimension.
Further, subtracting the mean value of a dimension variable from each spectrum matrix and dividing the mean value by the standard deviation of the dimension to complete the spectrum matrix EiThe data normalization process of (1).
Further, the data matrix obtained by performing data normalization processing on the relative density numerical value matrix F is recorded as Fi(n×p)，p＝1。
Furthermore, the data standardization processing of the relative density numerical value matrix can be completed by subtracting the mean value of a dimension variable from each relative density numerical value matrix and dividing the mean value by the standard deviation of the dimension.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a method for measuring relative density of tobacco essence perfume, which comprises obtaining a spectrogram of the tobacco essence perfume and a relative density value of the tobacco essence perfume to obtain a spectrum matrix and a relative density numerical matrix of a perfume sample, establishing a relative density model of the tobacco essence perfume based on a partial least square method according to the spectrum matrix and the relative density numerical matrix, obtaining a spectrum matrix component and a relative density numerical matrix component of the spectrum matrix and the relative density numerical matrix which accord with the maximum variance through the partial least square method, then obtaining the spectrum matrix component and the relative density numerical matrix component of the residual main component quantity in sequence by removing the spectrum matrix component and the residual error matrix which accord with the maximum variance, establishing a corresponding mathematical model of the relative density value and the spectrogram of the tobacco essence perfume according to all the obtained spectrum matrix component and relative density numerical matrix component, the method is simple, can continuously measure the flavors and fragrances of different brands, can accurately obtain the spectrogram of the tobacco flavor and fragrance by the spectrometry, has high detection precision, and can quickly and accurately realize the determination of the relative density content of the tobacco flavor and fragrance.
Furthermore, an infrared spectrogram of the essence and the spice is obtained by adopting an infrared test, so that the detection speed is high, and the accuracy is high.
Furthermore, the relative density value of the tobacco flavor and fragrance is rapidly detected by using the Raman spectrum, and the accuracy is high.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is an infrared spectrum of a sample of the tobacco flavor and fragrance of example 1 of the present invention.
FIG. 3 is a Raman spectrum of a tobacco flavor sample in example 2 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
as shown in figure 1, the method for measuring the relative density of the tobacco flavor and fragrance comprises the following steps:
step 1), obtaining a spectrogram of a flavor and fragrance sample, and obtaining a spectral matrix E of the flavor and fragrance sample according to the obtained spectrogram;
specifically, dripping a flavor sample on an optical bench to perform infrared test or Raman test to obtain an infrared spectrogram or Raman spectrogram of the flavor for the cigarette;
specifically, a mid-infrared test or a near-infrared test is adopted, and the parameters of a spectrometer adopting the near-infrared test are as follows: the scanning times are 4-256 times, and the resolution is 4cm-1～64cm-1Wavelength range of 10000cm-1～4000cm-1(ii) a The spectrometer parameters for mid-infrared testing were: the scanning times are 2-256 times, and the resolution is 1cm-1～64cm-1Wavelength range 4000cm-1～400cm-1(ii) a IntoSpectrometer parameters for the row raman test were: the scanning times are 2-64 times, the integration time is 500-5000 ms, and the wavelength range is 152cm-1～2488cm-1。
The spectrum collection mode comprises attenuation total reflection, transmission, diffuse reflection and diffuse transmission reflection;
step 2), obtaining the relative density value of the essence and spice sample, and establishing a relative density numerical matrix F of the essence and spice sample according to the relative density value of the essence and spice sample;
specifically, a density refractometer is adopted to measure the relative density value and the refractive index value of the essence and spice for the cigarettes;
step 3), respectively establishing relative density models of the tobacco flavors and fragrances based on a partial least square method: combining the spectrum matrix and the relative density numerical matrix of the essence and spice sample to establish a relative density model of the essence and spice for the cigarette;
firstly, carrying out data standardization processing on the spectrum matrix E to obtain the spectrum matrix E after standardization processingi(nxm), wherein n is the number of samples, and m is the dimensionality;
the data matrix obtained after the data standardization processing is carried out on the relative density numerical value matrix F is recorded as Fi(n×p，p＝1)；
Specifically, the method comprises the following steps: and (3) carrying out data standardization processing on the spectral matrix E: that is, the mean value of one dimension variable subtracted from each spectrum matrix is divided by the standard deviation of the dimension to complete the spectrum matrix EiThe data standardization processing of (2);
specifically, the method comprises the following steps: carrying out data standardization processing on the relative density numerical value matrix F: that is, the mean value of a dimension variable subtracted from each relative density numerical matrix is divided by the standard deviation of the dimension to complete the relative density numerical matrix FiThe data standardization processing of (2);
in the spectral matrix EiExtracting the spectral matrix component tiIn a matrix of relative density values FiExtracting relative density numerical value matrix component ui；
Relative density matrix of values FiIn particular to a relative density value and relative density numerical matrix of a flavor and fragrance sample;
the spectrum matrix EiAs an independent variable matrix, each row is a spectrum, and each column is a dimension variable;
matrix F of relative density valuesiAs a dependent variable matrix, a matrix of relative density values FiOnly one column;
calculating the spectral matrix component t meeting the maximum varianceiAnd relative density numerical matrix component uiNamely:
Cov(ti,ui)–>max；
cov is the covariance sign, max is the maximum sign;
spectral matrix component tiIs a spectral matrix EiLinear combination of, i.e. ti＝EiWi+1，Wi+1Is a spectral weight coefficient, and similarly, a relative density numerical matrix component uiIs a relative density numerical matrix FiLinear combination of (1), ui＝FiCi+1，Ci+1Is a numerical weight coefficient, Wi+1And Ci+1The same is a unit vector;
establishing spectral matrix components tiAnd relative density numerical matrix component uiThe maximum variance of (c) is expressed as:
max<EiWi+1,FiCi+1>
Wi+1is a matrix Ei＇FiFi＇EiThe eigenvector corresponding to the largest eigenvalue, Ci+1Is a matrix Fi＇EiEi＇Fi+1The maximum eigenvector corresponding to the maximum eigenvalue can be solved by Lagrange to obtain Wi+1And Ci+1Value, Wi+1And Ci+1Are uniformly unitized, wherein | | Wi+1||＝1；||Ci+1||＝1,i≥0；
According to the acquired Wi+1And Ci+1The spectrum matrix component t with the maximum variance is obtained by inverse solutioniAnd relative density numerical matrix component ui(ii) a According to the acquired spectral matrix component tiAnd relative density numerical matrixComponent uiEstablishing a regression equation:
according to the obtained spectral matrix component tiEstablishing a spectral matrix EiSpectral residual matrix E ofi-1For the spectral matrix component tiAccording to the component u of the matrix of the relative density valuesiEstablishing a relative density numerical matrix FiNumerical residual matrix F ofi-1For relative density numerical matrix component uiThe regression equation of (a):
Ei-1＝ti×p’i+Ei
Fi-1＝ui×q’i+Fi
Fi-1＝ti×r’i+Fi
in the formula, piIs a spectral matrix EiOf the ith load vector, qiIs a relative density numerical matrix FiOf the ith load vector, riIs tiAnd uiThe relationship vector of (1); ei-1Is a spectral matrix EiSpectral residual matrix of (F)i-1Is a relative density numerical matrix FiThe numerical residual matrix of (2);
the regression coefficient vector is calculated as follows:
spectral residual matrix Ei-1I.e. from the spectral matrix EiRemoving solved spectral matrix component tiThe residual spectrum matrix and the numerical residual error matrix Fi-1I.e. from the relative density value matrix FiRemoving solved relative density numerical matrix component uiResidual relative density afterA matrix of values;
from the spectral residual matrix E, respectivelyi-1Sum value residual error matrix Fi-1Extracting the spectral matrix component t meeting the maximum variance requirementi-1And relative density numerical matrix component ui-1Establishing a spectrum residual error matrix Ei-1Spectral residual matrix E ofi-2For the spectral matrix component ti-1To establish a numerical residual matrix Fi-1Numerical residual matrix F ofi-2For relative density numerical matrix component ui-1To obtain a spectrum residual error matrix Ei-2Sum value residual error matrix Fi-2Repeating the above steps to obtain the spectral matrix component ti-nRelative density matrix component ui-nSpectrum residual matrix Ei-nSum value residual error matrix Fi-n，nThe relative density main component quantity;
spectral residual matrix Ei-2I.e. from the spectral matrix Ei-1Removing solved spectral matrix component ti-1The residual spectrum matrix and the numerical residual error matrix Fi-2I.e. from the relative density value matrix Fi-1Removing solved relative density numerical matrix component ui-1The remaining relative density numerical matrix;
according to the acquired spectral matrix component ti-nAnd relative density numerical matrix component ui-nEstablishing a spectral matrix EiAnd relative density numerical matrix FiThe regression expression of (1):
Ei＝tip’i+ti-1p’i-1+...+tAp’A
Fi＝tir’i+ti-1r’i-1+...+tAr’A+FA
a is a spectral matrix EiAnd a matrix of relative density values FiThe rank of (d); t is t1,…,tARepresents E1，E2，…，EAThe linear combination of (a) and (b),
obtaining the expression of relative density:
in the formula, y*Is a relative density value, F(i-n)kAs a numerical residual matrix Fi-nThe kth line of (1); wherein { ak1,ak2,...,akmThe values of the regression coefficients are obtained; x is the number of1，x2，…，xmThe infrared spectrum data value of the essence and spice to be detected is obtained; and substituting the spectral data value of the essence and spice to be detected into the relative density expression to obtain the relative density value of the essence and spice to be detected.
According to the invention, the relative density value of the sample to be tested can be calculated and obtained by obtaining the spectrogram data of the sample to be tested and using the formula based on the spectrogram data, and meanwhile, the refractive index value of the tobacco flavor can be tested by using the method.
And (3) verification process:
the modeling accuracy was evaluated by the correction decision coefficient (R2_ Cal), the prediction decision coefficient (R2_ Pre), the cross validation Root Mean Square Error (RMSECV), and the prediction Root Mean Square Error (RMSEP):
r2_ Cal and R2_ PRE are calculated as follows:
the RMSECV calculation is as follows:
the RMSEP calculation formula is as follows:
in the formula, yi,actualThe relative density and refractive index measured values of the essence and flavor for the tobacco are tested or verified in the ith test set;
is the average of the measured values of all samples in the method; y isi,predictedThe method is a prediction value of the ith sample in the prediction process, n is the spectrum number of the sample in the test set, and m is the spectrum number of the sample in the verification set. Generally, the closer R2_ Cal and R2_ Pres are to 1, the better, the closer RMSECV and RMSEP are to 0, the better.
Example 1
The adopted equipment Agilent Cary 630 Fourier transform intermediate infrared spectrometer and the test sample spectrum accessory liquid measurement technology Dialpath transmission method have the optical path of 30 mu m and the wavelength range of 4000-650 cm-1. The resolution of the instrument is 4cm-1The number of scanning times is 32, and the types of the tobacco flavors and fragrances participating in modeling are 59.
As shown in figure 2, the three-time repeated results of the spectrum of the tobacco flavor sample can show that the repeated spectrum in a part of wave number intervals has the phenomenon of large absorbance deviation, and in order to enhance the robustness of the model, the area with large absorbance deviation is removed. And establishing a relation between the spectral data and the actually measured data of the reference method corresponding to the spectral data by using a partial least square module. The calibration set is used for establishing a model, the prediction set is used for verifying the model, and the model is evaluated according to four indexes of R2_ Cal, R2_ Pre, RMSECV and RMSEP, and the results are shown in the following table 1. It can be found that R2_ Cal and R2_ Pre are close to 1, and RMSECV and RMSEP are close to 0, which indicates that when the spectrum is not processed by the preprocessing method, the correction set model has good prediction effect and high prediction accuracy.
TABLE 1
Example 2
The adopted equipment comprises the following steps: portable raman spectrometer with 1064nm laser, obstetrician: b is&W TEK, a Raman fiber probe attached to a test sample spectrum, and a diffuse reflection method. Wavelength range of 152cm-1～2488cm-1. The instrument integration time was 5000ms and the number of scans was 4. The total amount of the flavor and fragrance for the cigarettes participating in modeling is 351 batches.
The Raman spectrum result of The tobacco flavor and fragrance sample is shown in figure 3, at The moment, The spectrum data is preprocessed by adopting standard normal variable transformation, and The relationship is established between The spectrum data (after being preprocessed) and The corresponding reference method data by using The partial least square module of The Unscamblebler. The calibration set is used for establishing a model, the verification set is used for verifying the model, and the model is evaluated according to four indexes of R2_ Cal, R2_ Pre, RMSECV and RMSEP, and the results are shown in the following table 2. It can be found that R2_ Cal and R2_ Pre are close to 1, and RMSECV and RMSEP are close to 0, which shows that when the spectrum is processed by the preprocessing method, the correction set model has good prediction effect and high prediction accuracy.
TABLE 2
According to the implementation cases, the invention provides a novel method for rapidly measuring the physical indexes of the tobacco essence perfume, which is used for controlling the quality of the tobacco essence perfume. Sampling and storing the tobacco essence perfume, and acquiring a mid-infrared spectrogram; measuring the physical index (relative density and refractive index) value of the tobacco flavor and fragrance by adopting a tobacco industry standard method; establishing a relation between the physical index and the spectral data by combining a partial least square method and taking the relation as a correction set model; samples not participating in modeling were used to predict their two index values. The model is verified by four indexes of R2_ Cal, R2_ Pre, RMSECV and RMSEP. The two examples show that the physical index prediction capability of the tobacco essence perfume is better through the mid-infrared spectroscopy, so that the physical index determination of the tobacco essence perfume can be rapidly, accurately and in situ realized.
Claims (10)
1. The method for measuring the relative density of the tobacco essence and flavor is characterized by comprising the following steps:
step 1), obtaining a spectrogram of a flavor and fragrance sample, and obtaining a spectral matrix E of the flavor and fragrance sample according to the obtained spectrogram;
step 2), obtaining the relative density value of the essence and spice sample, and establishing a relative density numerical matrix F of the essence and spice sample according to the relative density value of the essence and spice sample;
step 3), establishing a relative density model of the tobacco essence perfume based on a partial least square method:
standardizing the spectrum matrix E to obtain the standardized spectrum matrix EiNormalizing the relative density numerical matrix F to obtain a normalized relative density numerical matrix FiIn the spectral matrix EiExtracting the spectral matrix component tiIn a matrix of relative density values FiExtracting relative density numerical value matrix component uiMaking the acquired spectral matrix component tiAnd relative density numerical matrix component uiThe maximum variance is met, i.e.:
Cov(ti,ui)–>max；
cov is the covariance sign, max is the maximum sign;
establishing spectral matrix components tiAnd relative density numerical matrix component uiMaximum variance expression of (2):
max<EiWi+1,FiCi+1>；
Wi+1is a spectral weight coefficient, Ci+1Is a numerical weight coefficient;
obtaining W through Lagrange solutioni+1And Ci+1Value, where Wi+1||＝1；||Ci+1||＝1,i≥0；
According to Wi+1And Ci+1The spectrum matrix component t with the maximum variance is obtained by inverse solutioniAnd relative density numerical matrix component ui；
According to the obtained spectral matrix component tiEstablishing a spectral matrix EiSpectral residual matrix E ofi-1For the spectral matrix component tiAccording to the component u of the matrix of the relative density valuesiEstablishing a relative density numerical matrix FiNumerical residual matrix F ofi-1For relative density numerical matrix component uiThe regression equation of (a):
Ei-1＝ti×p’i+Ei
Fi-1＝ui×q’i+Fi
Fi-1＝ti×r’i+Fi
wherein:
in the formula, piIs a spectral matrix EiOf the ith load vector, qiIs a relative density numerical matrix FiOf the ith load vector, riIs tiAnd uiThe relationship vector of (1);
obtaining a spectrum residual error matrix E according to the abovei-1Sum value residual error matrix Fi-1Obtaining a spectral matrix component ti-nRelative density matrix component ui-nSpectrum residual matrix Ei-nSum value residual error matrix Fi-n，nThe relative density main component quantity;
according to the acquired spectral matrix component ti-nAnd relative density numerical matrix component ui-nEstablishing a spectral matrix EiAnd relative density numerical matrix FiThe regression expression of (1):
Ei＝tip’i+ti-1p’i-1+...+tAp’A
Fi＝tir’i+ti-1r’i-1+...+tAr’A+FA
a is a spectral matrix EiAnd a matrix of relative density values FiThe rank of (d); t is t1,…,tARepresents E1，E2，…，EAOfThe combination of the characters is that the characters of the character,
obtaining the expression of relative density:
in the formula, y*Is a relative density value, F(i-n)kAs a numerical residual matrix Fi-nThe kth line of (1); wherein { ak1,ak2,...,akmThe values of the regression coefficients are obtained; x is the number of1，x2，…，xmThe infrared spectrum data value of the essence and spice to be detected is obtained; and substituting the spectral data value of the essence and spice to be detected into the relative density expression to obtain the relative density value of the essence and spice to be detected.
2. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 1, wherein in step 1), the tobacco flavor and fragrance sample is dropped on an optical bench to perform an infrared test or a Raman test, so as to obtain an infrared spectrum or a Raman spectrum of the tobacco flavor and fragrance.
3. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 2, wherein the infrared test comprises a near infrared test and a mid-infrared test, and the parameters of a spectrometer adopting the near infrared test are as follows: the scanning times are 4-256 times, and the resolution is 4cm-1～64cm-1Wavelength range of 10000cm-1～4000cm-1(ii) a The spectrometer parameters for mid-infrared testing were: the scanning times are 2-256 times, and the resolution is 1cm-1～64cm-1Wavelength range 4000cm-1～400cm-1。
4. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 2, wherein the parameters of a spectrometer for performing Raman test are as follows: the scanning times are 2-64 times, the integration time is 500-5000 ms, and the wavelength range is 152cm-1～2488cm-1。
5. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 2, wherein the spectrum collection mode comprises attenuated total reflection, transmission, diffuse reflection and diffuse transflection.
6. The method for measuring the relative density of the flavor and fragrance for the cigarettes as claimed in claim 1, wherein in step 2), a density refractometer is used to measure the relative density value and the refractive index value of the flavor and fragrance for the cigarettes.
7. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 1, wherein in the step 3), the spectral matrix E is subjected to data standardization treatment to obtain the standardized spectral matrix Ei(n × m), n is the number of samples, and m is the dimension.
8. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 7, wherein the spectral matrix E is obtained by subtracting the mean value of a dimension variable from each spectral matrix and dividing the mean value by the standard deviation of the dimensioniThe data normalization process of (1).
9. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 1, wherein the data matrix F after the data standardization processing is performed on the numerical matrix F of the relative density is recorded as Fi(n×p)，p＝1。
10. The method for measuring the relative density of the tobacco flavor and fragrance as claimed in claim 9, wherein the data standardization of the relative density numerical matrix is completed by subtracting the mean value of a dimension variable from each relative density numerical matrix and dividing the mean value by the standard deviation of the dimension.
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