Methods for analyzing the causes of quality fluctuations in reconstituted tobacco leaves

Abstract

This invention discloses a method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves, comprising: conducting thermogravimetric analysis (TGA) experiments on the reconstituted tobacco leaf sample to be analyzed and a reference reconstituted tobacco leaf sample, respectively, to obtain the differential thermogravimetric analysis (DGA) curves of the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample, namely, the S1 curve and the S2 curve; calculating the difference in the derivative thermogravimetric values ​​of the S1 curve and the S2 curve within the intervals of the abscissa A1, A2, A3, and A4, where A1 is 35℃~133℃, A2 is 133℃~225℃, A3 is 225℃~597℃, and A4 is 597℃~760℃; and determining the cause of the quality fluctuations in reconstituted tobacco leaves based on the calculation results. The method provided by this invention can help quickly identify the cause of quality fluctuations in reconstituted tobacco leaves.

Description

Technical Field

[0001] This invention relates to the field of reconstituted tobacco quality control methods, and in particular to a method for analyzing the causes of quality fluctuations in reconstituted tobacco. Background Technology

[0002] Reconstituted tobacco is a sheet-like raw material for tobacco products, made from tobacco leaves, stems, and other raw materials through a papermaking process. The manufacturing process involves first soaking the tobacco leaves and other raw materials in water, then separating the extract containing tobacco components from the tobacco pulp containing insoluble substances such as fibers. The tobacco pulp is then processed using papermaking technology and equipment to form a base sheet, which is then coated with a coating solution and dried to become a sheet-like reconstituted tobacco. Reconstituted tobacco is a high-value-added product of tobacco resource recycling. Blending it into cigarettes can significantly reduce consumption per carton, improve cigarette structure and combustion, and reduce the release of tar and harmful components in cigarette smoke. In recent years, reconstituted tobacco has become an indispensable and important component of cigarette products, participating in the combustion process. Currently, the standard used for delivery inspection and supervision of reconstituted tobacco products is "YC / T 16-2014 Reconstituted Tobacco." Ensuring the quality stability of reconstituted tobacco is crucial for maintaining the quality stability of cigarette products. During the processing and production process, the quality of reconstituted tobacco products may sometimes fluctuate. When quality fluctuations occur, it is important to quickly identify the cause of the fluctuations to ensure the stability of the quality of reconstituted tobacco products. Summary of the Invention

[0003] The purpose of this invention is to provide a method that can help quickly find the cause of quality fluctuations when reconstituted tobacco leaves exhibit quality fluctuations.

[0004] This invention discloses a method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves, comprising:

[0005] Thermogravimetric analysis experiments were conducted on the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample to obtain the differential thermogravimetric analysis curves of the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample, namely the S1 curve and the S2 curve.

[0006] The differences in the differential thermogravimetric values ​​of curves S1 and S2 within the intervals A1, A2, A3 and A4 on the horizontal axis are calculated respectively, where A1 is 35℃~133℃, A2 is 133℃~225℃, A3 is 225℃~597℃ and A4 is 597℃~760℃.

[0007] Based on the calculation results, determine the reasons for the fluctuations in the quality of reconstituted tobacco leaves.

[0008] In some embodiments, determining the cause of quality fluctuations in reconstituted tobacco leaves includes:

[0009] When the difference in the thermogravimetric values ​​of the micro-merchant within the A1 interval is the largest, the reason for the quality fluctuation is determined to be the large difference in the percentage of moisture content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample.

[0010] When the difference in thermogravimetric values ​​of micro-entrants within the A2 range is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of coating material mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample.

[0011] When the difference in the thermogravimetric values ​​of the micro-merchant within the A3 range is the largest, the reason for the quality fluctuation is determined to be the large difference in the percentage of substrate material mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample.

[0012] When the difference in the micro-thermogravimetric values ​​within the A4 range is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of calcium carbonate mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample.

[0013] In some embodiments, calculating the difference between the S1 curve and the S2 curve in the intervals A1, A2, A3, and A4 includes:

[0014] Take n1 points for both curves S1 and S2 within interval A1. The x-coordinates of these n1 points are identical for both curves S1 and S2. Then, calculate the degree of difference between curves S1 and S2 within interval A1 using the following formula:

[0015]

[0016] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point among n1 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. is the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE is the degree of difference, in %;

[0017] Take n² points for both curves S1 and S2 within interval A2, ensuring that the x-coordinates of these n² points correspond identically. Then, calculate the degree of difference between curves S1 and S2 within interval A2 using the following formula:

[0018]

[0019] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n2 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. is the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE is the degree of difference, in %;

[0020] Take n3 points for both curves S1 and S2 within interval A3. The x-coordinates of these n3 points are identical for both curves S1 and S2. Then, calculate the degree of difference between curves S1 and S2 within interval A3 using the following formula:

[0021]

[0022] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n3 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. is the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE is the degree of difference, in %;

[0023] Take n4 points for both curves S1 and S2 within interval A2. The x-coordinates of the n4 points for curves S1 and S2 are identical. Then, calculate the degree of difference between curves S1 and S2 within interval A4 using the following formula:

[0024]

[0025] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n4 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let NRMSE be the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE be the degree of difference, expressed in %.

[0026] In some embodiments, the values ​​of n1, n2, n3, and n4 are the same, and the x-coordinates of the n1 points divide the A1 interval into n1+2 intervals on average, the x-coordinates of the n2 points divide the A2 interval into n2+2 intervals on average, the x-coordinates of the n3 points divide the A3 interval into n3+2 intervals on average, and the x-coordinates of the n4 points divide the A4 interval into n4+2 intervals on average.

[0027] In some embodiments, thermogravimetric analysis experiments are performed on the reconstituted tobacco leaf sample to be analyzed and a reference reconstituted tobacco leaf sample, respectively, including:

[0028] When performing thermogravimetric analysis on the reconstituted tobacco sample to be analyzed, take more than 35g of the reconstituted tobacco sample to be analyzed and grind it into powder with a particle size of less than 40 mesh. Then, take 15mg of the powder from the ground sample for thermogravimetric analysis.

[0029] When conducting thermogravimetric analysis on the reference reconstituted tobacco sample, take more than 35g of the reference reconstituted tobacco sample and grind it into powder with a particle size of less than 40 mesh. Then, take 15mg of the powder from the ground sample for thermogravimetric analysis.

[0030] In some embodiments, thermogravimetric analysis experiments are performed on the reconstituted tobacco leaf sample to be analyzed and a reference reconstituted tobacco leaf sample, respectively, including:

[0031] When performing thermogravimetric analysis (TGA) experiments on the reconstituted tobacco leaf samples to be analyzed and the reference reconstituted tobacco leaf samples, the TGA experimental conditions were set as follows: nitrogen was used as the ambient gas, the ambient gas flow rate was 40 mL / min, the heating rate was 20 °C / min, and the starting and ending temperatures of the TGA experiments were 30 °C and 800 °C, respectively.

[0032] In some embodiments, the coating material includes fragrance, flavoring, tobacco leaf extract and / or tobacco stem extract, and the substrate material includes cellulose, lignin and hemicellulose.

[0033] Based on the method for analyzing the causes of quality fluctuations in reconstituted tobacco provided by this invention, thermogravimetric analysis (TGA) experiments are conducted on a reference reconstituted tobacco sample and a reconstituted tobacco sample exhibiting quality fluctuation problems. Differential thermogravimetric analysis (DGA) curves for the reconstituted tobacco sample to be analyzed and those for the reference reconstituted tobacco sample are obtained. The degree of difference between the reference reconstituted tobacco sample and the reconstituted tobacco sample to be analyzed within the temperature ranges of 35℃~133℃, 133℃~225℃, 225℃~597℃, and 597℃~760℃ is calculated based on the curves. The magnitude of this degree of difference can determine the cause of the quality fluctuations.

[0034] Other features and advantages of the invention will become clear from the following detailed description of exemplary embodiments of the invention with reference to the accompanying drawings. Attached Figure Description

[0035] The accompanying drawings, which are included to provide a further understanding of the invention and form part of this application, illustrate exemplary embodiments of the invention and, together with their description, serve to explain the invention and do not constitute an undue limitation thereof. In the drawings:

[0036] Figure 1 This is a flowchart of the method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves according to an embodiment of the present invention;

[0037] Figure 2 This is a schematic diagram of the TG and DTG curves of the reconstituted tobacco leaf samples used in the thermogravimetric analysis experiment according to an embodiment of the present invention. Detailed Implementation

[0038] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0039] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps set forth in these embodiments do not limit the scope of the invention. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.

[0040] In the description of this invention, it should be understood that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore should not be construed as limiting the scope of protection of this invention.

[0041] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0042] For ease of description, spatial relative terms such as "above," "on top of," "on the upper surface of," "above," etc., are used herein to describe the spatial positional relationship of a device or feature as shown in the figures to other devices or features. It should be understood that spatial relative terms are intended to encompass different orientations in use or operation beyond the orientation of the device as described in the figures. For example, if the device in the figures were inverted, a device described as "above" or "on top of" other devices or structures would subsequently be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below." The device may also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein will be interpreted accordingly.

[0043] Thermogravimetric analysis (TGA), also known as thermogravimetry (TG), is a thermal analysis technique that measures the relationship between the mass of a substance and temperature (w = f(T)) under programmed temperature control. For example... Figure 2 As shown, the curve obtained by thermogravimetric analysis is called the TG curve or TGA curve, with temperature on the horizontal axis and mass percentage on the vertical axis. The differential thermogravimetric analysis curve, also known as the derivative thermogravimetric analysis (DTG) curve, is obtained by taking the first derivative of the TG curve with respect to temperature (the vertical axis is dm / dT (also known as the derivative thermogravimetric value), and the horizontal axis is temperature; its physical meaning represents the relationship between the rate of weight loss and temperature).

[0044] like Figure 1 As shown, the method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves in this embodiment includes:

[0045] S100: Thermogravimetric analysis (TGA) experiments were performed on the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample, respectively, to obtain the differential thermogravimetric analysis (DGA) curves for the sample to be analyzed and the reference reconstituted tobacco leaf sample, i.e., curves S1 and S2. The reference reconstituted tobacco leaf sample is the reconstituted tobacco leaf sample used as a quality standard, while the sample to be analyzed is the reconstituted tobacco leaf sample exhibiting quality fluctuations. When analyzing the reasons for the quality fluctuations of the reconstituted tobacco leaf sample that exhibits quality fluctuations relative to the quality standard, a sample of the reconstituted tobacco leaf sample exhibiting quality fluctuations was taken as the sample to be analyzed, and a sample of the reconstituted tobacco leaf sample used as the quality standard was taken as the reference reconstituted tobacco leaf sample. Thermogravimetric analysis experiments were performed on both types of samples, and the DGA curves for each type of sample were obtained. The DGA curve for the sample to be analyzed is curve S1, and the DGA curve for the reference reconstituted tobacco leaf sample is curve S2.

[0046] S200 calculates the difference in derivative thermogravimetric values ​​for curves S1 and S2 within the intervals A1, A2, A3, and A4 on the abscissa, where A1 is 35℃~133℃ (308K~406K Kelvin), A2 is 133℃~225℃ (406K~498K Kelvin), A3 is 225℃~597℃ (498K~870K Kelvin), and A4 is 597℃~760℃ (870K~1033K Kelvin). After obtaining curves S1 and S2, the difference in derivative thermogravimetric values ​​between curves S1 and S2 within the four temperature intervals A1, A2, A3, and A4 is calculated.

[0047] S300, based on the difference in the differential thermogravimetric values ​​within the four intervals A1, A2, A3 and A4, determines the cause of the quality fluctuation of reconstituted tobacco leaves.

[0048] The inventors discovered through experiments that when sensory evaluations of reconstituted tobacco products show fluctuations in taste and other sensory qualities, the cause of these fluctuations can be analyzed by examining the substances lost during thermogravimetric analysis (TGA) of the reconstituted tobacco products within the temperature ranges of 35℃~133℃, 133℃~225℃, 225℃~597℃, and 597℃~760℃. The percentage of mass lost at these temperatures corresponds to the percentage of moisture, coating material, substrate material, and calcium carbonate content in the reconstituted tobacco sample, respectively. By calculating and comparing the differences within these temperature ranges, the cause of the quality fluctuations can be determined.

[0049] When the difference in the differential thermogravimetric values ​​within the A1 interval is the largest, the reason for the quality fluctuation is determined to be the large difference in the percentage of moisture content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. In other words, the large difference in the water content ratio between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample is the main reason for the difference in the reconstituted tobacco sample to be analyzed compared to the reference reconstituted tobacco sample. When the difference in the thermogravimetric values ​​of the micro-quotient within the A2 interval is the largest, the cause of the quality fluctuation is judged to be a large difference in the percentage of coating material content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. In other words, the large difference in the proportion of coating material in the reconstituted tobacco sample to be analyzed compared with the reference reconstituted tobacco sample is the main reason for the difference in quality between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. The coating material refers to the substance added to the coating liquid during the manufacturing process of the reconstituted tobacco sample and finally adhered to the reconstituted tobacco sample after being coated onto the substrate. The large difference in the percentage of coating material content may be due to differences in the composition of the coating liquid during the manufacturing of different reconstituted tobacco samples, differences in the adhesion effect of the coating liquid, etc. After analyzing the cause, the coating process of the reconstituted tobacco can be further examined to further refine and clarify the cause of the quality fluctuation of the reconstituted tobacco. When the difference in the differential thermogravimetric values ​​within the A3 interval is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of substrate material content between the reconstituted tobacco sample and the reference reconstituted tobacco sample. In other words, the significant difference in the proportion of substrate material mass between the reconstituted tobacco sample and the reference sample is the main reason for the quality fluctuation. The substrate material is used to adhere the coating material and mainly includes cellulose, lignin, and hemicellulose. When the difference is large within the A3 interval, the percentage of cellulose, lignin, and hemicellulose mass content can be analyzed to determine the cause of the quality fluctuation. When the difference in the differential thermogravimetric values ​​within the A4 interval is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of calcium carbonate mass content between the reconstituted tobacco sample and the reference reconstituted tobacco sample. Calcium carbonate is an important additive in the papermaking reconstituted tobacco process and is also an important component of papermaking reconstituted tobacco. When smoking cigarettes, calcium carbonate burns along with the reconstituted tobacco. Different mass percentages of calcium carbonate participating in combustion have significantly different effects on the sensory quality of reconstituted tobacco. When the difference in the micro quotient thermogravimetric value in the A4 range is the greatest, it can be determined that the difference in calcium carbonate content is an important reason for the quality fluctuation of reconstituted tobacco.

[0050] In some embodiments, calculating the difference between the S1 curve and the S2 curve in the intervals A1, A2, A3, and A4 includes:

[0051] Take n1 points within interval A1 for both curves S1 and S2. The x-coordinates of these n1 points correspond one-to-one with the x-coordinates of the points on both curves S1 and S2. That is, the temperature values ​​at the n1 different points on the S1 curve and the n1 different points on the S2 curve within interval A1 correspond one-to-one. Then, calculate the degree of difference between curves S1 and S2 within interval A1 using the following formula:

[0052]

[0053] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point among n1 points. Let be the differential thermogravimetric value at the i-th point in the S1 curve, which is the ordinate value of the i-th point in the S1 curve. Let NRMSE be the differential thermogravimetric value at the i-th point in the S2 curve, i.e., the ordinate value of the i-th point in the S2 curve. NRMSE is the degree of difference, in percentage.

[0054] Take n² points for both curves S1 and S2 within interval A2. The x-coordinates of these n² points are identical for both curves, meaning the temperature values ​​at the n² different points on curve S1 and curve S2 within interval A2 are identical. Then, calculate the degree of difference between curves S1 and S2 within interval A2 using the following formula:

[0055]

[0056] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n2 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let NRMSE be the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE be the degree of difference, expressed in %.

[0057] Take n3 points for both curves S1 and S2 within interval A3. The x-coordinates of these n3 points correspond one-to-one with the x-coordinates of the curves S1 and S2, meaning the temperature values ​​of the n3 different points on the S1 curve and the S2 curve within interval A3 correspond one-to-one. Then calculate the degree of difference between curves S1 and S2 within interval A3 using the following formula:

[0058]

[0059] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n3 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let NRMSE be the differential thermogravimetric value at the i-th point in the S2 curve, and NRMSE be the degree of difference, expressed in %.

[0060] Take n4 points for both curves S1 and S2 within interval A2. The x-coordinates of these n4 points correspond one-to-one with the x-coordinates of the curves S1 and S2, meaning the temperature values ​​of the n4 different points on the S1 curve and the S2 curve within interval A4 correspond one-to-one. Then calculate the degree of difference between curves S1 and S2 within interval A4 using the following formula:

[0061]

[0062] Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n4 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let be the differential thermogravimetric value of the i-th point in the S2 curve, and NRMSE be the difference degree in percentage. The values ​​of n1, n2, n3, and n4 can be the same or different, meaning that the number of points taken in the four intervals A1, A2, A4, and A4 for either the S1 or S2 curve can be the same or different. However, for both the S1 and S2 curves, the number of points taken in the four intervals A1, A2, A4, and A4 must be the same, and the x-coordinate values ​​of the points must be equal.

[0063] In some embodiments, after calculating the difference between the S1 and S2 curves of each interval according to the above formula, the calculated values ​​can be directly compared. In some embodiments, each calculated value can be multiplied by a weighting coefficient before comparison. The value of the weighting coefficient is obtained based on experimental and empirical values. For example, regarding the influence of reconstituted tobacco on taste, the influence of coating material, cellulose, lignin, hemicellulose, calcium carbonate, and moisture content decreases successively. Therefore, the difference calculation result of the corresponding A2 interval is multiplied by the largest weighting coefficient before comparison, the difference calculation result of the corresponding A3 interval is multiplied by the second largest weighting coefficient before comparison, the difference calculation result of the corresponding A4 interval is multiplied by the second largest weighting coefficient before comparison, and the difference calculation result of the corresponding A1 interval is multiplied by the smallest weighting coefficient before comparison. In some embodiments, the weighting coefficients of the difference calculation values ​​in the four intervals A1, A2, A4, and A4 before comparison are 0.6, 1, 0.8, and 0.7, respectively.

[0064] In some embodiments, the values ​​of n1, n2, n3, and n4 are the same, and the x-coordinates of n1 points divide the A1 interval into n1+2 equal intervals, the x-coordinates of n2 points divide the A2 interval into n2+2 equal intervals, the x-coordinates of n3 points divide the A3 interval into n3+2 equal intervals, and the x-coordinates of n4 points divide the A4 interval into n4+2 equal intervals. That is, in this embodiment, the number of points taken from each individual S1 curve or S2 curve within the four intervals A1, A2, A4, and A4 is the same, and the x-coordinates of the multiple points taken within each interval equally divide the interval. The point selection method in this embodiment makes the obtained data more representative and improves the accuracy of the data.

[0065] In some embodiments, thermogravimetric analysis experiments are performed on the reconstituted tobacco leaf sample to be analyzed and a reference reconstituted tobacco leaf sample, respectively, including:

[0066] When performing thermogravimetric analysis on the reconstituted tobacco sample to be analyzed, take more than 35g of the reconstituted tobacco sample to be analyzed and grind it into powder with a particle size of less than 40 mesh. Then, take 15mg of the powder from the ground sample for thermogravimetric analysis.

[0067] When conducting thermogravimetric analysis (TGA) on a reference reconstituted tobacco sample, a sample of at least 35g was taken and ground into powder with a particle size of less than 40 mesh. Then, 15mg of the ground powder was taken for TGA analysis. This embodiment, by taking at least 35g of reconstituted tobacco sample for grinding, ensures that the powder is more uniform and representative, while the 15mg sample size meets the requirements for TGA analysis.

[0068] In some embodiments, thermogravimetric analysis experiments are performed on the reconstituted tobacco leaf sample to be analyzed and a reference reconstituted tobacco leaf sample, respectively, including:

[0069] When performing thermogravimetric analysis (TGA) experiments on the reconstituted tobacco leaf samples to be analyzed and the reference reconstituted tobacco leaf samples, the TGA experimental conditions were set as follows: nitrogen was used as the ambient gas, the ambient gas flow rate was 40 mL / min, the heating rate was 20 °C / min, and the starting and ending temperatures of the TGA experiments were 30 °C and 800 °C, respectively.

[0070] In some embodiments, the coating material includes fragrance, flavoring, tobacco leaf extract and / or tobacco stem extract, and the substrate material includes cellulose, lignin and hemicellulose.

[0071] The invention is illustrated below with two different embodiments:

[0072] Example 1

[0073] Two reconstituted tobacco products with significant differences in sensory evaluation, namely Product A and Product B, were obtained. Table 1 shows the sensory evaluation scores of Product A and Product B given by seven sensory experts. The sensory evaluation scores for Product A and Product B were 92.64 and 88.70, respectively, indicating a large difference in sensory quality. The similarity of the thermogravimetric curves of Product A and Product B analyzed using common thermal analysis methods (e.g., the method disclosed in Chinese Patent Application No. 201711326629.5) was 94.40%, indicating that the two products were very similar. The reason for the difference in sensory evaluation between these two products is unclear. The present invention will be used to investigate and analyze the reasons for the difference in sensory evaluation between the two products.

[0074] Table 1 Summary of Sensory Evaluation Scores

[0075]

[0076] According to the method of the present invention, more than 35g of product A sample is taken and ground into powder with a particle size of less than 40 mesh. Then, 15mg of the powder is taken for thermogravimetric analysis. The thermogravimetric analysis is performed using a NETZSCH TG209 F3 simultaneous thermal analyzer (NETZSCH GmbH, Germany). Nitrogen is used as the ambient gas, the ambient gas flow rate is 40mL / min, the heating rate is 20℃ / min, and the starting and ending temperatures of the thermogravimetric analysis are 30℃ and 800℃, respectively. Similarly, more than 35g of product B sample is taken and ground into powder with a particle size of less than 40 mesh. Then, 15mg of the powder is taken for thermogravimetric analysis. Based on the experimental results, differential thermal gravimetric analysis curves of products A and B were obtained. Then, based on the curves, the differences between products A and B in the four intervals A1, A2, A3, and A4 were calculated to be 3.40%, 18.91%, 3.50%, and 2.39%, respectively. Therefore, it was concluded that the reason for the difference in sensory evaluation between the two products was that the percentage of substrate material mass content, calcium carbonate mass content, and moisture mass content were relatively similar, but the percentage of coating material mass content differed significantly.

[0077] After learning the cause of the quality fluctuation, the reconstituted tobacco manufacturer was notified to focus on checking the coating process and the extraction process of the coating solution. It was found that the original B product had slightly thinner flakes after coating than the A product. After trying to adjust the coating solution concentration and the number of coatings, the production was restarted. According to the method of this invention, the difference between the A product and the modified B product in the four intervals A1, A2, A3, and A4 was calculated to be 2.48%, 4.47%, 2.96%, and 1.95%, respectively. The difference between the A product and the modified B product in the four intervals A1, A2, A3, and A4 was generally close. Then, the original seven sensory evaluation experts were invited to conduct a sensory evaluation again. The results are shown in Table 2. The B product scored 91.56 in the sensory evaluation after the improvement. The expert group believed that the improvement effect was obvious, and the overall difference between the two groups of products was significantly reduced, which is consistent with the present invention.

[0078] Table 2 Summary of Sensory Evaluation Scores

[0079]

[0080] Example 2

[0081] A reconstituted tobacco plant reported that the sensory evaluation of some batches of reconstituted tobacco products produced at the beginning and end of the year differed significantly from expectations, and assistance was needed to identify the cause of the product quality fluctuations. The quality stability of this specification of reconstituted tobacco produced by the plant in the beginning and end quarters of the year was tracked; product information is shown in Table 3.

[0082] Table 3 Reconstituted Tobacco Product Information Table

[0083]

[0084] Based on conventional thermal analysis methods, and using the first batch of qualified samples from the first quarter as a benchmark for comparison, it can be concluded that there are indeed two batches of products in the fourth quarter with significantly different similarities to their thermogravimetric curves. The results are shown in Table 4.

[0085] Table 4. Similarity Results of Reconstituted Tobacco Products

[0086] Comparison Products Z11 Z12 Z13 Z14 Z15 Z41 Z42 Z43 Z44 Z45 Similarity (%) 100 97.776 98.549 98.33 97.497 98.569 93.899 97.95 77.776 97.823

[0087] The method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves of the present invention was used to calculate the degree of difference between different batches of reconstituted tobacco leaf products and the first batch of qualified samples in the first quarter in the four intervals A1, A2, A3, and A4.

[0088] According to the method of this invention, the same thermogravimetric analysis (TGA) experiment was performed on each batch of products in each quarter, taking product Z12 as an example. A sample of product Z12 weighing more than 35g was ground into powder with a particle size less than 40 mesh. Then, 15mg of the ground powder was taken for TGA analysis. The TGA analysis was performed using a NETZSCH TG209 F3 simultaneous thermal analyzer (NETZSCH GmbH, Germany), with nitrogen as the ambient gas. The ambient gas flow rate was 40mL / min, and the heating rate was 20℃ / min. The starting and ending temperatures of the TGA experiment were 30℃ and 800℃, respectively. Differential thermogravimetric analysis (DGA) curves for each batch of products were obtained based on the experiment. Then, the differences between each batch of products and the first batch of qualified samples in the first quarter in the four intervals A1, A2, A3, and A4 were calculated based on the curves. The results are shown in Table 5.

[0089] Table 5 Results of the weighted differences in reconstituted tobacco products (%)

[0090] Comparison Products Phase 1 Phase 2 Phase 3 Phase 4 Z11 0 0 0 0 Z12 7.715 1.552 1.975 0.895 Z13 4.719 2.669 1.201 0.462 Z14 9.567 2.468 2.187 0.847 Z15 6.195 3.845 1.562 0.557 Z41 10.195 3.206 1.971 0.962 Z42 10.839 20.063 4.530 1.056 Z43 8.707 2.546 1.411 0.724 Z44 250.493 18.400 8.899 1.615 Z45 11.605 1.781 2.025 1.289

[0091] According to the calculation results, the sensory evaluation of the second batch of reconstituted tobacco products in the fourth quarter showed quality fluctuations due to a significant difference in the percentage of coating material content compared to the first batch of products in the first quarter, and the fourth batch of products in the fourth quarter showed a significant difference in the percentage of moisture content compared to the first batch of products in the first quarter.

[0092] According to the method of the present invention, the quality fluctuation of reconstituted tobacco products was analyzed, and the reconstituted tobacco manufacturers were notified to check whether there were any uncleaned water stains on the production line and the equipment status of the coating process section. After inspection of the production records, it was found that the production of the fourth batch of products in the fourth quarter was rushed. The production line was not allowed to dry completely after cleaning, which led to a large deviation in the moisture content of the reconstituted tobacco products. After strengthening management, the relevant problems have not occurred again.

[0093] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications can still be made to the specific implementation of the present invention or equivalent substitutions can be made to some technical features without departing from the spirit of the technical solutions of the present invention, and all such modifications and substitutions should be covered within the scope of the technical solutions claimed in the present invention.

Claims

1. A method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves, characterized in that, include: Thermogravimetric analysis experiments were conducted on the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample to obtain the differential thermogravimetric analysis curves of the reconstituted tobacco leaf sample to be analyzed and the reference reconstituted tobacco leaf sample, namely the S1 curve and the S2 curve. The differences in the differential thermogravimetric values ​​of curves S1 and S2 within the intervals A1, A2, A3 and A4 on the horizontal axis are calculated respectively, where A1 is 35℃~133℃, A2 is 133℃~225℃, A3 is 225℃~597℃ and A4 is 597℃~760℃. Based on the calculation results, the causes of quality fluctuations in reconstituted tobacco leaves were determined, including: When the difference in the thermogravimetric values ​​of the micro-merchant within the A1 interval is the largest, the reason for the quality fluctuation is determined to be the large difference in the percentage of moisture content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. When the difference in thermogravimetric values ​​of micro-enterprises within the A2 range is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of coating material mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. When the difference in the thermogravimetric values ​​of the micro-merchant within the A3 interval is the largest, the cause of the quality fluctuation is determined to be the large difference in the percentage of substrate material mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample. When the difference in the micro-thermogravimetric values ​​within the A4 range is the largest, the cause of the quality fluctuation is determined to be a large difference in the percentage of calcium carbonate mass content between the reconstituted tobacco sample to be analyzed and the reference reconstituted tobacco sample.

2. The method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves as described in claim 1, characterized in that, The differences between curves S1 and S2 within intervals A1, A2, A3, and A4 were calculated, including: Take n1 points for both curves S1 and S2 within interval A1. The x-coordinates of these n1 points are identical for both curves S1 and S2. Then, calculate the degree of difference between curves S1 and S2 within interval A1 using the following formula: , Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point among n1 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let be the derivative thermogravimetric value at the i-th point in the S2 curve. The degree of difference is expressed as a percentage. Take n² points for both curves S1 and S2 within interval A2, ensuring that the x-coordinates of these n² points correspond one-to-one with those of curves S1 and S2. Then, calculate the degree of difference between curves S1 and S2 within interval A2 using the following formula: Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n2 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let be the derivative thermogravimetric value at the i-th point in the S2 curve. The degree of difference is expressed as a percentage. Take n3 points for both curves S1 and S2 within interval A3. The x-coordinates of these n3 points are identical for both curves S1 and S2. Then, calculate the degree of difference between curves S1 and S2 within interval A3 using the following formula: Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n3 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let be the derivative thermogravimetric value at the i-th point in the S2 curve. The degree of difference is expressed as a percentage. Take n4 points for both curves S1 and S2 within interval A4. The x-coordinates of the n4 points for curves S1 and S2 are identical. Then, calculate the degree of difference between curves S1 and S2 within interval A4 using the following formula: Where m is the mass percentage of the remaining substance in the thermogravimetric analysis experiment at the current temperature, T is the temperature of the thermogravimetric analysis experiment, and point i is the i-th point out of n4 points. Let be the derivative thermogravimetric value at the i-th point in the S1 curve. Let be the derivative thermogravimetric value at the i-th point in the S2 curve. The degree of difference is expressed in percent.

3. The method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves as described in claim 1, characterized in that, Thermogravimetric analysis experiments were performed on the reconstituted tobacco leaf samples to be analyzed and the reference reconstituted tobacco leaf samples, including: When performing thermogravimetric analysis on the reconstituted tobacco sample to be analyzed, take more than 35g of the reconstituted tobacco sample to be analyzed and grind it into powder with a particle size of less than 40 mesh. Then, take 15mg of the powder from the ground sample for thermogravimetric analysis. When conducting thermogravimetric analysis on the reference reconstituted tobacco sample, take more than 35g of the reference reconstituted tobacco sample and grind it into powder with a particle size of less than 40 mesh. Then, take 15mg of the powder from the ground sample for thermogravimetric analysis.

4. The method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves as described in claim 1, characterized in that, Thermogravimetric analysis experiments were performed on the reconstituted tobacco leaf samples to be analyzed and the reference reconstituted tobacco leaf samples, including: When performing thermogravimetric analysis (TGA) experiments on the reconstituted tobacco leaf samples to be analyzed and the reference reconstituted tobacco leaf samples, the TGA experimental conditions were set as follows: nitrogen was used as the ambient gas, the ambient gas flow rate was 40 mL / min, the heating rate was 20℃ / min, and the starting and ending temperatures of the TGA experiments were 30℃ and 800℃, respectively.

5. The method for analyzing the causes of quality fluctuations in reconstituted tobacco leaves as described in claim 1, characterized in that, The coating material includes fragrances, flavorings, tobacco leaf extracts and / or tobacco stem extracts, and the substrate material includes cellulose, lignin and hemicellulose.

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