CN111307724A - Method for establishing model for determining cut stem content in cut tobacco based on color difference method - Google Patents
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Abstract
The invention relates to a method for establishing a model for determining the content of cut stems in cut tobacco based on a color difference method, which comprises the steps of preparing cut stems and cut leaves into powder respectively to prepare tobacco powder with different cut stem contents, and measuring the CIE-L of each test sample by using a color difference meter after each test sample is fully and uniformly mixed*a*b*The method is simple and rapid in operation, low in cost, high in accuracy and precision, good in repeatability and suitable for measuring the cut stem content in the cut tobacco in the formula.
Description
Technical Field
The invention belongs to the technical field of cut tobacco detection, and particularly relates to a method for determining cut stem content in cut tobacco in a formula based on a color difference method.
Background
The cigarette formula cut tobacco generally comprises cut tobacco leaves, cut stems and reconstituted cut tobacco leaves, and the stability of the content of each component has great influence on the smoking quality of cigarette products. In recent years, cut stems play more and more important roles in reducing cigarette harmfulness, regulating and controlling cigarette smoke level, improving application efficiency of tobacco leaf raw materials and the like, and the use proportion of the cut stems in a formula and the blending uniformity of the cut stems in cigarette cigarettes are more and more emphasized. Therefore, the method for accurately measuring the cut stem content in the cut tobacco is a key for judging and evaluating the effective utilization rate and blending quality of the cut stems, and is also widely concerned by technical and quality detection personnel in the industry.
In the past, the actual proportion of cut stems in cut tobacco in a formula is usually obtained by adopting manual visual observation or selecting and weighing by means of a visual amplification system according to the difference of morphological characteristics and colors of the cut stems. Although the method is simple to operate, the method has the defects of long time consumption, large artificial influence, inapplicability to mass detection and the like.
With the continuous development of the cut stem manufacturing technology, the morphological characteristics of the produced cut stems and cut leaves have smaller and smaller differences, and the selection by artificial vision becomes increasingly difficult. In addition, the apparent densities of the cut tobacco leaves, the cut stems and the reconstituted tobacco cut tobacco are similar, so that the cut tobacco leaves, the cut stems and the reconstituted tobacco cut tobacco cannot be separated by utilizing the difference of the densities. Meanwhile, the problems of small sample discrimination and poor repeatability in the determination process caused by the problems of the test method such as the chemical component difference of the tobacco raw materials or the industrial analysis difference are not enough to achieve the purpose of accurately determining the cut stem content in the cut tobacco.
In order to solve the problem, related researchers respectively adopt a uniform design-PLS-NIR method and a thermal analysis technology to predict the cut stem content in the cut tobacco formula. However, both methods are highly demanding on instrumentation and data processing and modeling are relatively complex.
Disclosure of Invention
The invention aims to provide a method for establishing a model for determining the content of cut stems in cut tobacco in formula based on a color difference method, so as to solve the problem of complex modeling for predicting the content of the cut stems in the cut tobacco in the formula in the prior art.
The invention is realized by the following technical scheme:
a method for establishing a model for determining cut stem content in cut tobacco based on a color difference method comprises the following steps:
h1, selecting cut stem samples and cut leaf samples, and processing the cut stem samples and the cut leaf samples into cut stem powder and cut leaf powder respectively;
h2, blending the cut stem powder and the cut leaf powder according to a set proportion to obtain Sn tobacco powder samples, wherein n is a natural number;
h3, selecting one tobacco powder sample from Sn tobacco powder samples, and measuring the color difference parameter L of the tobacco powder sample by using a color difference meter*、a*、b*Value of wherein L*Is from black to white, and represents a lightness value a*From green to red, representing the redness value, b*Selecting N different parts for measuring the tobacco powder samples from blue to yellow to represent a yellowness value, wherein N is a natural number larger than 2, and automatically calculating an average value for 1 time every N times of continuous measurement by a colorimeter, wherein each tobacco powder sample obtains Mn average values, and N is a natural number; then carrying out secondary average on the Mn average values to respectively obtain L*、a*、b*A value;
h4, and color difference parameter L obtained by measuring pure leaf shredded tobacco powder according to the mode of step H3*、a*And b*The values are base values, respectively L0、a0And b0And calculating a color difference value △ E according to a color difference formula:
H5, drawing and carrying out regression analysis by using the cut stem content and △ E to obtain a linear regression model of the cut stem content and the △ E value, wherein y is a △ E + b, y is the cut stem content, △ E is the color difference value, and a and b are constants.
Further, the cut stems are selected at a cut stem flavoring outlet, and the cut leaves are selected at a cut leaf drying and cooling outlet.
Further, the step H1 includes respectively drying the selected cut stems and cut leaves in an oven at 45 ℃ for 2H, crushing the cut stems and the cut leaves by a cyclone mill, and sieving the crushed cut stems and the cut leaves by a sieve with the aperture of 250 mu m to respectively obtain cut stem sample powder and cut leaf sample powder; and respectively placing the cut stem sample powder and the cut leaf sample powder in a constant-temperature and constant-humidity box with the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-2% for balancing for 48 hours to obtain the cut stem powder and the cut leaf powder.
Further, the specific determination method in step H3 includes the following steps:
1) putting a set amount of tobacco powder sample into a transparent container, pressing and flattening the tobacco powder sample to ensure that the tobacco powder sample does not loose and fall off after the transparent container is inverted, and then inverting the transparent container;
2) determination of L of a tobacco powder sample at the bottom of a transparent container using a colorimeter*、a*、b*A value;
3) and selecting a natural number with N being more than 2 at the bottom of the transparent container, automatically calculating an average value for 1 time by the color difference meter every N times of continuous measurement, wherein the measurement times of each tobacco powder sample are N x Mn times, and obtaining Mn average values, wherein N is the natural number.
Further, after the step H5, the method further includes an accuracy verification of the linear regression model of the cut rolled stems content and △ E value, and includes the following steps:
mixing the cut stem powder and the cut leaf powder to obtain P groups of test samples with different cut stem contents, and respectively determining the L of each test sample*、a*、b*And calculating △ E value according to a color difference formula, substituting the △ E value into a linear regression model of the cut stem content and the △ E value, calculating a theoretical value of the cut stem content, comparing the theoretical value with an actual value of the cut stem content in the test sample to obtain a relative error, and determining that the linear regression model of the cut stem content and the △ E value meets set requirements if the relative error is within a set range.
The invention has the beneficial effects that:
according to the technical scheme, by establishing the method for determining the cut stem content model in the cut tobacco based on the color difference method, the tobacco stems and the tobacco leaves have great difference in the appearance color of the finally prepared cut stems and cut leaves due to the great difference in the content and the proportion of internal chemical components such as plastid pigment, and the like, and the difference can be accurately quantified and characterized by using a color difference meter, so that the theoretical basis is laid for predicting the cut stem content in the cut tobacco based on the color difference method.
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FIG. 1 is a graph showing the variation trend of cut stem content and △ E value and a regression equation.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
In a batch of production time, cross section sampling is respectively carried out at a cut stem perfuming outlet and a cut leaf drying and cooling outlet, sampling is carried out for 1 time at intervals of 5min, each time is about 0.5kg, and sampling is carried out for 8 times, so that 4kg of each of a cut stem sample and a cut leaf sample is obtained. Uniformly mixing in a laboratory, then placing 0.5kg of cut stems and 1.5kg of cut leaves in a 45 ℃ oven for drying for 2h, crushing by using a cyclone mill, sieving by using a 60-mesh sieve with the aperture of 250 mu m to respectively obtain cut stem sample powder and cut leaf sample powder, and placing the obtained cut stem sample powder and the obtained cut leaf sample in a constant-temperature and constant-humidity box with the temperature of (22 +/-1) DEG C and the relative humidity of (60 +/-2)% for balancing for 48h to obtain cut stem powder and cut leaf powder. Blending the cut stem powder and the shredded tobacco powder according to the scheme in the table 1 to obtain tobacco powder samples with different cut stem contents, and placing each tobacco powder sample in a closed container to be fully and uniformly mixed.
TABLE 1 tobacco powder samples blended with cut stem powder and shredded tobacco powder
| Sample numbering | Cut rolled stems (g) | Cut tobacco (g) | Cut stem content (%) |
| S1 | 0 | 100.0 | 0 |
| S2 | 2.5 | 97.5 | 2.5 |
| S3 | 5.0 | 95.0 | 5.0 |
| S4 | 7.5 | 92.5 | 7.5 |
| S5 | 10.0 | 90.0 | 10.0 |
| S6 | 12.5 | 87.5 | 12.5 |
| S7 | 15.0 | 85.0 | 15.0 |
| S8 | 17.5 | 82.5 | 17.5 |
| S9 | 20.0 | 80.0 | 20.0 |
| S10 | 22.5 | 77.5 | 22.5 |
| S11 | 25.0 | 75.0 | 25.0 |
| S12 | 30.0 | 70.0 | 30.0 |
| S13 | 40.0 | 60.0 | 40.0 |
| S14 | 50.0 | 50.0 | 50.0 |
| S15 | 100.0 | 0 | 100.0 |
Taking about 10g of tobacco powder sample in each time of any tobacco powder sample, placing the tobacco powder sample in a quartz cup, compacting and flattening the tobacco powder sample by a sample presser as much as possible to ensure that the quartz cup does not loose and fall off after inversion, slowly inverting the quartz cup, and measuring the CIE-L of the tobacco powder sample at the bottom of the quartz cup by using a DC-P3 type full-automatic colorimeter*a*b*Color space value, where L*Is from black to white, and represents a lightness value, a*Is from green to red, represents the redness value, b*The yellowness values are expressed from blue to yellow. Selecting 3 different positions for measuring the tobacco powder sample in each quartz cup, automatically calculating 1 average value every 3 continuous measurements by a color difference meter, and sampling the tobacco powder samples with different cut stem ratios for 20 times for measurement, namely recording 20L of each tobacco powder sample*、a*、b*Value of, another 20L*、a*、b*The values are subjected to secondary average to obtain the L of the tobacco powder samples respectively*、a*、b*The value is obtained. The main technical indexes of the color difference meter are set according to the method in the literature.
The pure leaf shredded tobacco powder is used according to stepsColor difference parameter L obtained by measuring in a step H3 manner*、a*And b*The values are base values, respectively L0、a0And b0And calculating a color difference value △ E according to a color difference formula:
Independent sample T test and paired T test analysis are carried out on related data by using IBM SPSS Statistics 19.0 software, drawing and regression analysis are carried out on the cut stem content and the color difference value △ E by using Microsoft Excel 2010, and a function model of the cut stem content and the color difference value is established.
The difference degree of the color difference between the cut stems and the cut leaves is the basis for measuring the cut stem content in the cut tobacco in the formula by using the color difference method, the feasibility of the method is determined, and the higher the difference of the color difference parameters between the cut stems and the cut leaves is, the higher the accuracy of the prediction result of the cut stem content is.
According to the experimental method, the 15 tobacco powder samples (S1-S15) with different cut stem contents are subjected to the color difference parameter L*、a*、b*The value is measured, the average value of the measurement result is taken, △ E is calculated according to the Hunter color difference formula on the basis of the color difference parameter of the pure-leaf shredded tobacco powder (the cut stem content is 0), and the result is shown in Table 2.
TABLE 2 different cut stem content samples L*、a*、b*Value measurement results and △ E value
Drawing and regression analysis are carried out by using the cut stem content and the Hunter color difference △ E value, and a linear regression model of the cut stem content and the △ E value is y-a △ E + b (y is the cut stem content, △ E is the color difference, a and b are constants), as shown in figure 1, the linear regression equation is y-8.8989 △ E-0.9571 (R is the color difference of the cut stem content, and R is the constant of the cut stem content and the △ E) shown in figure 120.9995), which shows that the degree of fitting of a linear regression model between the cut stem content and the △ E value is high, and the correlation between the two reaches a very significant level (p is 0.000), and the larger the Hunter color difference △ E is, the higher the cut stem content is.
According to the experimental method, 5 groups of samples S16-S20 with different cut stem contents are prepared by using cut stem powder and cut leaf powder, and L of the samples is respectively measured after the samples are fully and uniformly mixed*、a*、b*The value is △ E value is calculated according to Hunter color difference formula, then the color difference △ E value of the sample to be measured is substituted into the linear model to calculate the cut stem content of the sample to be measured, the measurement result is shown in Table 3. As shown in Table 3, the relative errors of the cut stem content and the actual value measured by the linear regression model adopted by the same tobacco powder sample are between 2.00% and 3.37%, and are all less than 5%, the accuracy of the linear regression model is higher, the measured values and the actual values of the 5 samples are subjected to pairing t test, and P is 0.637 and is more than 0.05, the two groups of data have no significant difference, which shows that the difference is based on the color difference parameter L*、a*、b*The value deduces the determination method of the cut stem content in the cut tobacco in the formula.
TABLE 3 accuracy verification results for working models
As can be seen from table 4: the method is adopted to carry out 6 times of parallel measurement on 5 tobacco powder samples S21-S25 respectively, the variation coefficients of the measured results of the cut stem contents of the samples 1-5 are between 1.98-2.72% and are all less than 5%, which shows that the precision of the method for measuring the cut stem content in the cut tobacco in the formula is high and meets the requirement of quantitative analysis.
And then the method is adopted to carry out 6 times of continuous measurement on a certain tobacco powder sample, the measurement results of the cut stem content are respectively 12.48%, 11.99%, 12.17%, 12.26%, 12.59% and 11.81%, the average value is 12.22%, the standard deviation is 0.29%, and the variation coefficient is 2.40%, which shows that the method has good repeatability and meets the requirement of quantitative analysis.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for establishing a model for measuring cut stem content in cut tobacco based on a color difference method is characterized by comprising the following steps:
h1, selecting cut stem samples and cut leaf samples, and processing the cut stem samples and the cut leaf samples into cut stem powder and cut leaf powder respectively;
h2, blending the cut stem powder and the cut leaf powder according to a set proportion to obtain Sn tobacco powder samples, wherein n is a natural number;
h3, selecting one tobacco powder sample from Sn tobacco powder samples, and measuring the color difference parameter L of the tobacco powder sample by using a color difference meter*、a*、b*Value of wherein L*Is from black to white, and represents a lightness value a*From green to red, representing the redness value, b*Selecting N different parts for measuring the tobacco powder samples from blue to yellow to represent a yellowness value, wherein N is a natural number larger than 2, and automatically calculating an average value for 1 time every N times of continuous measurement by a colorimeter, wherein each tobacco powder sample obtains Mn average values, and N is a natural number; then carrying out secondary average on the Mn average values to respectively obtain L*、a*、b*A value;
H4and measuring the obtained color difference parameter L by using the pure-leaf shredded tobacco powder according to the step H3*、a*And b*The values are base values, respectively L0、a0And b0And calculating a color difference value △ E according to a color difference formula:
H5, drawing and carrying out regression analysis by using the cut stem content and △ E to obtain a linear regression model of the cut stem content and the △ E value, wherein y is a △ E + b, y is the cut stem content, △ E is the color difference value, and a and b are constants.
2. The method for establishing the model for measuring the cut stem content in the cut tobaccos based on the color difference method according to claim 1, wherein the cut stems are selected from a cut stem flavoring outlet, and the cut leaves are selected from a cut leaf drying and cooling outlet.
3. The method for establishing the stem content model in cut tobacco based on color difference method according to claim 1, wherein the step H1 further comprises drying the selected stem and cut tobacco in an oven at 45 ℃ for 2H, pulverizing with a cyclone mill, sieving with a sieve with a pore size of 250 μm to obtain stem sample powder and cut tobacco sample powder, respectively; and respectively placing the cut stem sample powder and the cut leaf sample powder in a constant-temperature and constant-humidity box with the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-2% for balancing for 48 hours to obtain the cut stem powder and the cut leaf powder.
4. The method for establishing the stem content model in the cut tobacco based on the color difference method according to claim 1, wherein the specific determination method in the step H3 comprises the following steps:
1) putting a set amount of tobacco powder sample into a transparent container, pressing and flattening the tobacco powder sample to ensure that the tobacco powder sample does not loose and fall off after the transparent container is inverted, and then inverting the transparent container;
2) determination of L of a tobacco powder sample at the bottom of a transparent container using a colorimeter*、a*、b*A value;
3) and selecting a natural number with N being more than 2 at the bottom of the transparent container, automatically calculating an average value for 1 time by the color difference meter every N times of continuous measurement, wherein the measurement times of each tobacco powder sample are N x Mn times, and obtaining Mn average values, wherein N is the natural number.
5. The method for establishing the stem content model in the cut tobacco based on the color difference method according to claim 1, wherein after the step H5, the method further comprises the accuracy verification of a linear regression model of the stem content and △ E value, and the method comprises the following steps:
mixing the cut stem powder and the cut leaf powder to obtain P groups of test samples with different cut stem contents, wherein P is a natural number, and respectively measuring L of each test sample*、a*、b*And calculating △ E value according to a color difference formula, substituting the △ E value into a linear regression model of the cut stem content and the △ E value, calculating a theoretical value of the cut stem content, comparing the theoretical value with an actual value of the cut stem content in the test sample to obtain a relative error, and determining that the linear regression model of the cut stem content and the △ E value meets set requirements if the relative error is within a set range.
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