CN113049438A - Method for rapidly identifying heat conversion characteristics of different tobaccos based on macroscopic quantity thermogravimetry - Google Patents
Method for rapidly identifying heat conversion characteristics of different tobaccos based on macroscopic quantity thermogravimetry Download PDFInfo
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Abstract
A method for rapidly identifying thermal conversion characteristics of different tobaccos based on a macro-thermogravimetry method is characterized in that a macro-thermogravimetry analyzer is used for obtaining weight loss curves of tobacco shreds at different constant temperatures; carrying out derivation on the weight loss curve to obtain a differential weight loss curve; selecting a proper standard base line, and obtaining a difference degree according to the comparison between a differential weightlessness curve of the tobacco shreds to be tested and the standard base line; numbering different tobacco shreds, selecting m temperature points for different samples to perform experiments, wherein each temperature point obtains a root mean square error RMSE (root mean square error) with a standard differential weight loss curve; for convenient calculation and marking, vectors are introduced
RMSE for each temperature point represents an element, which can be expressed as
The difference between the thermal conversion characteristics of different tobaccos can be obtained by operating different vectors. The invention introduces multiple temperaturesThe root mean square error of the degree points enables the one-dimensional data to form multi-dimensional data in a vector form, and differences among raw materials are analyzed through model length contrast, so that data difference sensitivity is improved, and the tobacco sample identification capability is improved.
Description
Technical Field
The invention belongs to the field of tobacco leaf formulas, and relates to a method for rapidly identifying heat conversion characteristics of different tobaccos based on a macroscopic quantity thermogravimetry method.
Background
In the production process of tobacco products, the formula of a tobacco leaf group can be influenced due to the shortage of certain tobacco leaf raw materials, and further, the production efficiency is reduced. In order to improve the production efficiency, reduce the inventory and maintain the leaf group formula, the difference between the tobacco leaves in inventory needs to be fully known. With the development of technology, various methods for identifying tobacco differences have been developed in the tobacco industry.
At present, methods for identifying differences between different tobaccos mainly comprise a modular formulation technology, near infrared spectrum detection, tobacco heat conversion characteristic difference degree analysis and the like.
The modular formula technology is used for carrying out differential analysis so as to produce cigarettes, the sensory experience of consumers can be more similar, but the formula personnel are required to deeply know the style and quality of tobacco leaves in each production place, and repeated smoking evaluation, comparison and adjustment are required.
The near infrared spectrum detection technology has the advantages of high speed, no damage, low cost and the like, but the difference degree between different samples obtained by the technology is small, and the difference generated in the scanning process can cover the difference between tobacco leaves, so the accuracy is poor.
The Chinese patent CN107860868A analyzes the heat conversion characteristics of different tobaccos through temperature programming and heat loss, the method is high in precision, but the sample form is only limited to the research of tobacco powder particles, and the research of Guo Gaifei and the like shows that the filling states and the material transfer processes of the tobacco powder particles and the tobacco shreds are greatly different. (study on the influence of the form of Guoguofei tobacco on its pyrolytic combustion characteristics and reaction kinetics [ D ]. Zhengzhou: Zhengzhou tobacco institute, 2019) therefore, the experiment using tobacco powder particles does not represent the properties of tobacco leaves well.
Disclosure of Invention
Aiming at the problems, the invention provides a method for rapidly identifying the difference of the heat conversion characteristics of different tobaccos, which utilizes a Chinese patent CN2854569Y tobacco wet heat treatment online analyzer (hereinafter referred to as a macro thermogravimetric analyzer) to carry out thermal weight loss analysis on the tobaccos under the constant temperature condition, does not need complex sample pretreatment and any chemical reagent, and has simple, convenient and rapid experimental process. Through the analysis of the tobacco thermal conversion characteristic difference, the tobacco pyrolysis difference degree can be represented through objective and quantitative data, and a beneficial reference is provided for the maintenance of the cigarette formula.
The purpose of the invention is realized by the following technical scheme:
a method for rapidly identifying thermal conversion characteristics of different tobaccos based on a macro-thermogravimetry method is characterized in that a macro-thermogravimetry analyzer is used for obtaining weight loss curves of tobacco shreds at different constant temperatures; carrying out derivation on the weight loss curve to obtain a differential weight loss curve; selecting a proper standard base line according to the differential of the tobacco shreds to be detectedComparing the weight loss curve with a standard base line to obtain a difference degree; numbering different cut tobaccos, e.g. samples 1, 2, 3; selecting m temperature points (three temperature points of 290 ℃, 450 ℃ and 550 ℃) for different samples to carry out experiments, wherein each temperature point obtains a root mean square error RMSE (root mean square error) with a standard differential weight loss curve; for convenient calculation and marking, vectors are introduced
Where n represents the sample number and the RMSE for each temperature point represents an element, which can be expressed as
The difference between different tobacco thermal conversion characteristics can be obtained by calculating different vectors, the vectors are introduced for calculation, and the single one-dimensional data is introduced to multiple dimensions, so that the sensitivity of the difference between the data is increased;
the variance is quantified and characterized using the root mean square error RMSE. RMSE is the normalized mean deviation of the true X and measured Y values, with RMSE closer to 0 indicating a smaller deviation of Y from X, and is expressed as:
where di is the deviation of the measured value from the true value, NmFor measuring times, the formula is introduced into the thermal conversion characteristics of tobacco for quantitative characterization, and reference sample data is defined as a true value X, target sample data is defined as a measured value Y, so di (dm/dt)i Target-(dm/dt)i DatumThe result is substituted into a formula,
in the formula: n is the number of points recorded by the macro thermogravimetric analyzer; i represents data of the ith point; t is time; (dm/dt) is the mass loss rate at a certain moment; (dm/dt)i TargetFor the tobacco sample to be testedThe experimental value of the product; (dm/dt)i DatumIs the experimental value of a reference tobacco sample;
the calculation formula of the vector modular length is
The closer the mode length obtained from the above formula is to 0, the closer the thermal conversion characteristics of the two are demonstrated.
The thermogravimetric analyzer can monitor the weight change of the tobacco shreds in the pyrolysis process in real time, feed data back to a computer through a sensor, plot the data to obtain a relation graph of time and weight, and derive the weight data with respect to time to obtain a differential weight loss curve.
The standard baseline is the differential thermogravimetric curve of the reference sample.
The tobacco shred sample has consistent shredding width, uniform length and uniform sample quality and stacking mode so as to ensure the repeatability of the experiment. Before the experiment, the sample was allowed to equilibrate in an oven at 105 ℃ for 20min to eliminate the effect of moisture.
The temperature control range of the macro thermogravimetric analyzer is 20-1000 ℃, and the temperature selection range is 105-900 ℃ according to the actual smoking process of tobacco products.
The atmosphere of the macro thermogravimetric analyzer can be set to be aerobic (air atmosphere) or anaerobic (nitrogen atmosphere); the adjustable range of the gas flow rate is 0-2000 mL/min.
The macro thermogravimetric analyzer refers to an on-line tobacco heat and humidity treatment analyzer of Chinese patent publication No. CN 2854569Y.
The invention has the following advantages:
1. the invention uses a self-developed macro thermogravimetric analyzer.
2. The sample form used by the invention is the tobacco shred, the sample amount is larger than that of the commercialized thermal weightlessness apparatus, and the Chinese patent CN107860868A uses the sample form as the tobacco powder, so that the pyrolysis process of the tobacco product in the actual stacking state can be accurately reflected by the application.
3. According to the invention, the thermal weight loss data is collected under the constant temperature condition, the sample is actually subjected to the rapid heating and constant temperature processes, and the Chinese patent CN107860868A adopts the programmed heating process, so that the application is close to the cigarette smoking process, and the data is more reliable.
4. The time for acquiring the sample weight loss data is far shorter than the temperature programmed in the Chinese patent CN107860868A, so the experimental process is simple, convenient and quick.
5. The method forms the one-dimensional data into the multi-dimensional data in a vector form by introducing the root mean square error of multiple temperature points, and analyzes the difference between the raw materials through the comparison of the model length, so that the sensitivity of the data difference is increased, and the capacity of identifying the tobacco samples is improved.
Drawings
FIG. 1 is a graph comparing differential thermogravimetric analysis at 290 ℃ in example 1,
FIG. 2 is a graph comparing differential thermogravimetric analysis at 450 ℃ in example 1,
FIG. 3 is a graph comparing differential thermogravimetric analysis at 550 ℃ in example 1,
FIG. 4 is a graph comparing differential thermogravimetric analysis at 290 ℃ in example 2,
FIG. 5 is a graph comparing differential thermogravimetric analysis at 450 ℃ in example 2,
FIG. 6 is a differential thermogravimetric comparison of example 2 at 550 ℃.
Detailed Description
The invention is further described by way of example with reference to the accompanying drawings:
example 1:
samples of experiment sample No. 168 (2018 Sichuan Liangshan Condong C3F) and No. 197 (2018 Yunnan Chuxiong C3F) were selected. The experimental conditions are as follows: the constant temperature was set at 290 ℃, 450 ℃ and 550 ℃ (the actual reaction furnace temperature was 30 ℃ lower than the set temperature), the flow rate of the reaction atmosphere nitrogen was 1000mL/min, and the flow rate of the shielding gas nitrogen was 500 mL/min. The sample is placed in an oven at 105 ℃ for 20min to remove water, and then 0.3000g +/-0.0005 g of the sample is weighed for pyrolysis. In order to ensure the accuracy of the experiment, two groups of parallel experiments are additionally arranged in each group of experiments, and the average value of three experiments is taken.
And performing first-order derivation on the obtained data to obtain a differential weight loss curve. FIGS. 1, 2 and 3 are views of respective drawingsIs a comparison graph of differential weight loss curves at 290 ℃, 450 ℃ and 550 ℃. Selecting a No. 168 sample as a reference sample, and calculating according to the RMSE formula, wherein the root mean square error values of the three temperature points are respectively 6.11 multiplied by 10-5、18.97×10-5、25.71×10-5For ease of calculation, all data is expanded by 105，
From the formula of the die length
From the above calculation results, it can be seen that there is a large difference in the thermal conversion characteristics of two different provinces of tobacco, which achieves similar results to the temperature programming method, but saves more time.
Example 2:
samples of test sample No. 117 (2017 Henan Luo Yang C3F) and No. 118 (2017 Henan Sanmenxia Luo C3F) were selected. The experimental conditions are as follows: the constant temperature was set at 290 ℃, 450 ℃ and 550 ℃ (the actual reaction furnace temperature was 30 ℃ lower than the set temperature), the flow rate of the reaction atmosphere nitrogen was 1000mL/min, and the flow rate of the shielding gas nitrogen was 500 mL/min. The sample is placed in an oven at 105 ℃ for 20min to remove water, and then 0.3000g +/-0.0005 g of the sample is weighed for pyrolysis. In order to ensure the accuracy of the experiment, two groups of parallel experiments are additionally arranged in each group of experiments, and the average value of three experiments is taken.
And performing first-order derivation on the obtained data to obtain a differential weight loss curve. FIGS. 4, 5 and 6 are graphs comparing differential weight loss curves at 290 deg.C, 450 deg.C and 550 deg.C, respectively. The No. 117 sample is selected as a standard sample and calculated according to the RMSE formula, and the root mean square error values of the three temperature points are respectively 2.0 multiplied by 10-5、8.1×10-5、13.9×10-5. To facilitate the calculation, all data is expanded 105，
From the formula of the die length
From the above calculation results, it can be obtained that the difference between the same province and different cities is obviously smaller than that between different provinces.
The results of the embodiment 1 and the embodiment 2 show that the heat conversion characteristics of different tobaccos are different, the tobacco leaves with larger difference have larger results, and the tobacco leaves with smaller difference have smaller results, so that the invention has certain reference value for replacing the tobacco leaves.
Claims (7)
1. A method for rapidly identifying heat conversion characteristics of different tobaccos based on a macroscopic quantity thermogravimetry method is characterized in that: obtaining weight loss curves of the cut tobacco at different constant temperatures through a macroscopic quantity thermogravimetric analyzer; carrying out derivation on the weight loss curve to obtain a differential weight loss curve; selecting a proper standard base line, and obtaining a difference degree according to the comparison between a differential weightlessness curve of the tobacco shreds to be tested and the standard base line; numbering different cut tobaccos, e.g. samples 1, 2, 3; selecting m temperature points for different samples to carry out experiments, wherein each temperature point obtains a root mean square error RMSE (root mean square error) with a standard differential weight loss curve; for convenient calculation and marking, vectors are introduced
Where n represents the sample number and the RMSE for each temperature point represents an element, which can be expressed as
The difference between different tobacco thermal conversion characteristics can be obtained by calculating different vectors, the vectors are introduced for calculation, and the single one-dimensional data is introduced to multiple dimensions, so that the sensitivity of the difference between the data is increased;
the difference is quantified and characterized by root mean square error RMSE, wherein RMSE refers to the normalized average deviation degree of a true value X and a measured value Y, the smaller the RMSE value is, the smaller the deviation of Y and X is, and the expression is as follows:
where di is the deviation of the measured value from the true value, NmFor measuring times, the formula is introduced into the thermal conversion characteristics of tobacco for quantitative characterization, and reference sample data is defined as a true value X, target sample data is defined as a measured value Y, so di (dm/dt)i Target-(dm/dt)i DatumThe substitution into the formula is carried out,
in the formula: n is the number of points recorded by the macro thermogravimetric analyzer; i represents data of the ith point; t is time; (dm/dt)i DatumIs the rate of mass loss at a time; (dm/dt)i TargetThe experimental value of the tobacco sample to be detected is obtained; (dm/dt)i DatumIs the experimental value of a reference tobacco sample;
the calculation formula of the vector modular length is
The closer the mode length obtained from the above formula is to 0, the closer the thermal conversion characteristics of the two are demonstrated.
2. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermogravimetric method as claimed in claim 1, wherein: the thermogravimetric analyzer can monitor the weight change of the tobacco shreds in the pyrolysis process in real time, feed data back to a computer through a sensor, plot the data to obtain a relation graph of time and weight, and derive the weight data with respect to time to obtain a differential weight loss curve.
3. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermogravimetric method as claimed in claim 1, wherein: the standard baseline is the differential thermogravimetric curve of the reference sample.
4. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermogravimetric method as claimed in claim 1, wherein: the tobacco shred sample has consistent shredding width, uniform length and uniform sample quality and stacking mode so as to ensure the repeatability of the experiment.
5. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermogravimetric method as claimed in claim 1, wherein: the temperature control range of the macro thermogravimetric analyzer is 20-1000 ℃, and the temperature selection range is 105-900 ℃ according to the actual smoking process of tobacco products.
6. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermogravimetric method as claimed in claim 1, wherein: the atmosphere of the macro thermogravimetric analyzer can be set to be an oxygen atmosphere, namely air atmosphere, or an oxygen-free atmosphere, namely nitrogen atmosphere; the adjustable range of the gas flow rate is 0-2000 mL/min.
7. The method for rapid identification of different tobacco thermal conversion characteristics based on the macrothermal method of claim 1 or 2 or 5 or 6, wherein: the macro thermogravimetric analyzer refers to an on-line tobacco heat and humidity treatment analyzer of Chinese patent publication No. CN 2854569Y.
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