CN114088581B - Method for detecting diffusion rate of applied feed liquid in heated cigarettes - Google Patents
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- CN114088581B CN114088581B CN202111284209.1A CN202111284209A CN114088581B CN 114088581 B CN114088581 B CN 114088581B CN 202111284209 A CN202111284209 A CN 202111284209A CN 114088581 B CN114088581 B CN 114088581B
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 90
- 238000009792 diffusion process Methods 0.000 title claims abstract description 45
- 239000007788 liquid Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 153
- 241000208125 Nicotiana Species 0.000 claims abstract description 90
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 90
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 238000002386 leaching Methods 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 5
- 238000004445 quantitative analysis Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000004817 gas chromatography Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000012527 feed solution Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 6
- 230000000391 smoking effect Effects 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract 1
- 238000000265 homogenisation Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 5
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 235000019437 butane-1,3-diol Nutrition 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The application relates to a method for detecting the diffusion rate of a material liquid applied to a heated cigarette, which comprises the steps of selecting reconstituted tobacco shreds for producing cigarettes and cigarettes produced by the reconstituted tobacco shreds, respectively detecting the glycerol content in the reconstituted tobacco shreds, the glycerol content on the tobacco shred surfaces at the center of the cigarettes and the glycerol content on the tobacco shred surfaces at 1/3 of the outer sides of the cigarettes by adopting a leaching method, and calculating the diffusion rate of the glycerol by adopting a formula. The detection method is convenient, the detection result is accurate and reliable, the detection method can be used for determining the shelf life of the heated cigarettes, improving the smoking experience, determining the homogenization evaluation time of the products and reducing the storage time.
Description
Technical Field
The application belongs to the technical field of detection of heated cigarettes, and particularly relates to a method for detecting the diffusion rate of a material liquid applied in a heated cigarette.
Background
With the rise of new tobacco in recent years, due to the lower hazard of the new tobacco, the new tobacco is gradually accepted by consumers in recent years, and especially a few consumers in foreign countries, and the heated cigarettes rapidly become new consumption hot spots in the cigarette market.
The orderly heating cigarette bar forming process is that tobacco leaf base paper or sheet coil with a certain width (100-160 mm) and added with fumigant is continuously unreeled by a unreeling device, the special sheet is conveyed to a shredding device by a conveying roller set, cut into tobacco bars with a certain width, the tobacco bars are gathered into bundles by a tobacco gathering device, the bundles are wrapped into cigarette bars by using forming paper, the cigarette bars are divided into cigarette cores with a certain length by a cigarette bar dividing device, and the cigarette cores and material functional sections are combined into cigarettes. For enriching smoke or creating heating cigarettes with different styles and tastes, a certain amount of feed liquid is usually applied by adopting a tape casting mode through a feed liquid applying device before tobacco shreds are gathered into a bundle, so that the applied feed liquid is generally at the central position of a tobacco section, and tobacco shreds which are directly contacted with the feed liquid in cigarettes only account for about 10% of the total amount of the tobacco shreds, and the feed liquid needs to be gradually and uniformly spread through natural diffusion of the feed liquid; because the boiling point of the heated cigarette feed liquid is generally higher, the diffusion speed is slower, and if the heated cigarette feed liquid does not reach a uniform state, the stability of the heated cigarette in mouth-by-mouth smoking can be affected. Therefore, how to detect the diffusion rate and uniformity of the feed liquid, judge the proper pumping time and determine the shelf life becomes a difficult problem which puzzles the product development, the improvement of the perfuming system and the shelf life. At present, a detection method for detecting the diffusion rate and uniformity of feed liquid in a heated cigarette is not found.
Disclosure of Invention
The application aims to provide a method for detecting the diffusion rate of a material liquid applied to a heated cigarette, so as to solve the problem that no detection method is available for the diffusion rate and uniformity of the material liquid.
In order to achieve the above purpose, the application is realized by the following technical scheme:
a method for detecting the diffusion rate of an applied feed liquid in a heated cigarette comprising the steps of:
s1, in a shredding process, sampling tobacco shreds in any batch in a random sampling mode to serve as a basic tobacco shred sample;
s2, in a cigarette production process, extracting cigarettes produced by the same batch of tobacco shreds as the basic tobacco shred sample in the step S1 as samples to be detected;
s3, averagely dividing the sample to be detected in the step S2 into M parts, wherein M is a natural number greater than 2, and respectively storing in a sealing way;
s4, after an interval of N hours from the time of extracting the sample to be detected, taking out the tobacco shred at the center of the cigarette and the tobacco shred at the set position in the first cigarette of the sample to be detected respectively, wherein the tobacco shred at the center of the cigarette is a center tobacco shred sample, and the tobacco shred at the set position is a set tobacco shred sample;
s5, respectively leaching a basic tobacco shred sample, a central tobacco shred sample and a set tobacco shred sample by adopting a leaching method to extract glycerol on the surface of the tobacco shred sample, respectively fixing the volume by using a methanol solution, and then quantitatively analyzing by using GC-MS to determine the content of the glycerol on the surface of the tobacco shred sample;
s6, the diffusion rate of the glycerol at the center of the cigarette and the diffusion rate of the glycerol at the set position are respectively as follows:
ei= (Ai-X)/(A0-X) X100%; es= (As-X)/(A0-X) ×100%; wherein Ei is the diffusion rate of glycerol at the center of a cigarette, es is the diffusion rate of glycerol at a set position, A0 is the theoretical content of glycerol in the feed liquid applied in the cigarette, ai is the glycerol content of the tobacco shred surface at the center of the cigarette, as is the glycerol content of the tobacco shred surface at the set position, X is the glycerol content in a base tobacco shred sample, and A0 is the glycerol content of the tobacco shred sample;
s7, calculating whether the value of Ei-Es is in a set range, and if so, applying a feed liquid diffusion rate of (Ai-X)/N (A0-X) multiplied by 100 percent; if not, entering S8;
s8, selecting a second sample to be detected, repeating the steps S4 to S7 after 2N hours from the time of extracting the sample to be detected, and applying the material liquid with the diffusion rate of (Ai-X)/2N (A0-X) multiplied by 100 percent, and circulating until the M sample to be detected is selected, wherein the diffusion rate of the material liquid is (Ai-X)/MN (A0-X) multiplied by 100 percent.
Further, the cut tobacco drawn from each part of the single cigarette is not more than 20mg.
Further, the specific steps of leaching in the step S5 are as follows:
weighing a cut tobacco sample with a set weight, placing the cut tobacco sample in a 500mL beaker, immersing the cut tobacco sample in 300mL of methanol for +/-2 s, filtering the cut tobacco sample, shaking up the filtrate, taking 20.0 mu L of methanol solution, and shaking up the supernatant of the filtrate to 1mL with constant volume.
Further, the methanol solution was 30.0g/L of 1, 3-butanediol internal standard methanol solution.
Further, in the quantitative analysis by GC-MS, a chromatographic column adopts a polar elastic quartz capillary column with the diameter of 30m multiplied by 0.25mm and the diameter of 0.25 mu m;
the gas chromatography conditions were: sample inlet temperature: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode;
mass spectrometry conditions: ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
The beneficial effects of the application are as follows:
the detection method of the technical scheme is convenient and fast, the detection result is accurate and reliable, the detection method can be used for determining the shelf life of the heated cigarettes, improving the smoking experience, and determining the time for evaluating the homogeneity of the products and reducing the storage time.
Drawings
FIG. 1 is a graph showing the change of glycerol content at different positions of a cigarette over storage time.
Detailed Description
The following examples are given by way of illustration only and are not to be construed as limiting the scope of the application.
According to the technical scheme, the tobacco material does not contain glycerol, and the glycerol applied to the raw material sheet is used for bringing the aroma substances out through vaporization and fogging to form aerosol, so that the smoking experience is met. The glycerol content in the raw material sheet is generally between 2 and 5% by weight, and the glycerol content in the applied feed liquid is used as a solvent and accounts for 30 to 50% of the total weight of the feed liquid, so that it is feasible to demonstrate the application of the feed liquid diffusion rate in the heated cigarettes by detecting the glycerol content.
The technical scheme provides a method for detecting the diffusion rate of a material liquid applied to a heated cigarette, which comprises the following steps:
s1, in the shredding process, any batch of tobacco shreds are sampled in a random sampling mode to serve as a basic tobacco shred sample, and because the cigarettes in the technical scheme are heated tobacco shreds formed by shredding prepared tobacco sheets, glycerol with a certain weight is usually added in the preparation process of the tobacco sheets so as to improve the fuming amount of the tobacco sheets, and the tobacco leaves do not usually contain glycerol.
S2, in the cigarette production process, the cigarette machine process or the pressing process is referred to herein, because the production of the existing heating type cigarette comprises two conditions of rolling and pressing, sampling is performed at this time, the tobacco shreds of the sampled cigarettes and the tobacco shreds of the basic tobacco shred samples are the same batch of tobacco shreds, otherwise, the data error is too large, the data error is not represented, the cigarette extraction mode is the same as the conventional cigarette detection extraction mode, the interval extraction or other extraction modes can be adopted, the realization of the technical scheme of the application is not influenced, and the extracted cigarettes are taken as the samples to be detected.
The sample to be detected is divided into M parts, wherein M is a natural number greater than 2, and in the technical scheme of the application, the sample to be detected can be divided into 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20 parts and the like, and the samples to be detected after the separation are respectively sealed and stored under the same condition without being listed one by one.
S4, from the time of sampling the sample to be tested, the interval is N hours, where N is a natural number, in the present application, N may be any desired value, such as 10 hours, 15 hours, 20 hours, 24 hours, 30 hours, 36 hours, etc., and in the following embodiments of the present application, N is exemplified as 24 hours. In this embodiment, after 24 hours of interval, the cut tobacco at the center of the cigarette and the cut tobacco at the set position in the first sample to be detected are respectively taken out, and the single cigarette is sealed for standby after each sampling of not more than 20mg at each position.
S5, improving the leaching method of the tobacco shred samples by referring to a method established by Severson and the like, wherein the specific steps are as follows: 15g (accurate to 0.0001 g) of tobacco shred samples are weighed, placed in a 500mL beaker, and immersed in 300mL of methanol, wherein the extraction time is controlled to be set value +/-2 s; filtering out cut tobacco, shaking the filtrate, taking 20.0 mu L of 1, 3-butanediol (internal standard) methanol solution with the concentration of 30.0g/L, fixing the volume to 1mL by using the supernatant of the filtrate, shaking the filtrate, carrying out quantitative analysis by using GC-MS, and determining the content of glycerol in the feed liquid on the surface of the cut tobacco.
Quantitative analysis was performed using an Agilent7890A-5973GC-MS gas chromatograph/mass spectrometer. (1) chromatography column: DB-WAX chromatographic column (30 m x 0.25mm,0.25 μm) polar elastic quartz capillary column. (2) gas chromatography conditions: sample inlet temperature: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode. (3) Mass Spectrometry conditions: ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
S6, after the cut tobacco with the feed liquid is coiled into a cigarette, the feed liquid at the center of the cigarette is diffused to the periphery, so that the glycerol content at the center of the cigarette is actually in a reduced state, the glycerol content of the cut tobacco at the set position is in an increased state, and in order to ensure the detection accuracy, the set position is usually selected in a range of 1/3 of the radius of the cigarette, which is equal to three equal parts and is close to the outer side of the cigarette, because if the radius is too close to the center of the cigarette, the concentration during diffusion is increased and then is reduced, the detection difficulty is increased, and the glycerol content of the cut tobacco at the outer 1/3 of the cigarette is in an increased state.
In each embodiment of the application, the set position is the tobacco shred at the outer 1/3 position of the cigarette and is taken as the detection position.
The diffusion rate of the glycerol at the center of the cigarette and the diffusion rate of the glycerol at the set position are respectively as follows:
ei= (Ai-X)/(A0-X) X100%; es= (As-X)/(A0-X) ×100%; ei is the diffusion rate of glycerol at the center of a cigarette, es is the diffusion rate of glycerol at a set position, A0 is the theoretical content of glycerol in the feed liquid applied to the cigarette, ai is the glycerol content of the surface of tobacco shreds at the center of the cigarette, as is the glycerol content of the surface of the tobacco shreds at the set position, X is the glycerol content of a base tobacco shred sample, and A0 is the glycerol content of mg/mL.
S7, calculating whether the value of Ei-Es is in a set range or not, in the normal case, when the value of Ei-Es is equal to 0 (theoretical value), the diffusion of the material liquid applied in the cigarette is completely uniform and is completed, the best suction experience state of the cigarette is processed, when the value of Ei-Es is larger than 0 but smaller, the diffusion of the material liquid applied is basically completed, and when the value of Ei-Es is larger than 0 but larger, the material liquid applied in the cigarette is in a rapid diffusion stage, and the material liquid is required to be stored continuously at the initial stage of the completion of the manufacture of the cigarette.
If the ratio is within the set range, the diffusion rate of the applied feed liquid is (Ai-X)/N (A0-X) multiplied by 100 percent; if not, entering S8;
s8, selecting a second sample to be detected, repeating the steps S4 to S7 after 2N hours (namely 48 hours) from the time of extracting the sample to be detected, and applying the material liquid with the diffusion rate of (Ai-X)/2N (A0-X) multiplied by 100 percent, and circulating until the M sample to be detected is selected, wherein the diffusion rate of the material liquid is (Ai-X)/MN (A0-X) multiplied by 100 percent.
As shown in fig. 1, the content of glycerol at different positions of a cigarette of a certain brand of heated cigarette changes with the storage time, and it can be seen from the drawing that the content of glycerol at different positions in the cigarette is close to that of glycerol at different positions after the cigarette is stored for 14 days to 16 days, and the content of glycerol at different positions is basically unchanged after 17 days. And then, the corresponding delivery is carried out by combining the approximate time from the start of the delivery of the heated cigarettes to the time of the delivery of the cigarettes in the hands of consumers, so that the warehouse occupation is reduced. For example, 3 days or more are required from the shipment to the customer, the storage time and the transfer time are more than or equal to 10 days, namely, the shipment can be carried out after the storage time is 7 days, and the shipment can be carried out on the production day if the time from the shipment to the customer is 14 days, so that the occupation of the warehouse can be reduced.
The present application is not limited to the above embodiments, but is not limited to the above embodiments, and any person skilled in the art will have obvious modifications and modifications equivalent to those of the equivalent embodiments, and can make various changes and modifications without departing from the scope of the present application.
Claims (6)
1. A method for detecting the diffusion rate of an applied feed liquid in a heated cigarette, comprising the steps of:
s1, in a shredding process, sampling tobacco shreds in any batch in a random sampling mode to serve as a basic tobacco shred sample;
s2, in a cigarette production process, extracting cigarettes produced by the same batch of tobacco shreds as the basic tobacco shred sample in the step S1 as samples to be detected;
s3, averagely dividing the sample to be detected in the step S2 into M parts, wherein M is a natural number greater than 2, and respectively storing in a sealing way;
s4, after an interval of N hours from the time of extracting the sample to be detected, taking out the tobacco shred at the center of the cigarette and the tobacco shred at the set position in the first cigarette of the sample to be detected respectively, wherein the tobacco shred at the center of the cigarette is a center tobacco shred sample, and the tobacco shred at the set position is a set tobacco shred sample;
s5, respectively leaching a basic tobacco shred sample, a central tobacco shred sample and a set tobacco shred sample by adopting a leaching method to extract glycerol on the surface of the tobacco shred sample, respectively fixing the volume by using a methanol solution, and then quantitatively analyzing by using GC-MS to determine the content of the glycerol on the surface of the tobacco shred sample;
s6, the diffusion rate of the glycerol at the center of the cigarette and the diffusion rate of the glycerol at the set position are respectively as follows:
ei= (Ai-X)/(A0-X) X100%; es= (As-X)/(A0-X) ×100%; wherein Ei is the diffusion rate of glycerol at the center of a cigarette, es is the diffusion rate of glycerol at a set position, A0 is the theoretical content of glycerol in the feed liquid applied in the cigarette, ai is the glycerol content of the tobacco shred surface at the center of the cigarette, as is the glycerol content of the tobacco shred surface at the set position, X is the glycerol content in a base tobacco shred sample, and A0 is the glycerol content of the tobacco shred sample;
s7, calculating whether the value of Ei-Es is in a set range, and if so, applying a feed liquid diffusion rate of (Ai-X)/N (A0-X) multiplied by 100 percent; if not, entering S8;
s8, selecting a second sample to be detected, repeating the steps S4 to S7 after 2N hours from the time of extracting the sample to be detected, and applying the material liquid with the diffusion rate of (Ai-X)/2N (A0-X) multiplied by 100 percent, and circulating until the M sample to be detected is selected, wherein the diffusion rate of the material liquid is (Ai-X)/MN (A0-X) multiplied by 100 percent.
2. The method of detecting a rate of diffusion of an applied liquid in a heated cigarette according to claim 1, wherein the individual cigarettes draw no more than 20mg of tobacco per cut.
3. The method for detecting the diffusion rate of an applied liquid in a heated cigarette according to claim 1, wherein the specific step of leaching in step S5 is:
weighing a cut tobacco sample with a set weight, placing the cut tobacco sample in a 500mL beaker, immersing the cut tobacco sample in 300mL of methanol for +/-2 s, filtering the cut tobacco sample, shaking up the filtrate, taking 20.0 mu L of methanol solution, and shaking up the supernatant of the filtrate to 1mL with constant volume.
4. The method of detecting the rate of diffusion of an applied feed solution in a heated cigarette according to claim 3, wherein the methanol solution is 30.0 g/L1, 3-butanediol internal standard methanol solution.
5. The method for detecting the diffusion rate of a material liquid applied to a heated cigarette according to claim 1, wherein in quantitative analysis by GC-MS, a chromatographic column is a polar elastic quartz capillary column of 30m×0.25mm and 0.25 μm;
the gas chromatography conditions were: sample inlet temperature: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode;
mass spectrometry conditions: ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
6. The method for detecting the diffusion rate of a liquid applied to a heated cigarette according to claim 1, wherein the set position is a detection position of cut tobacco at 1/3 of the outer side of the cigarette.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB0916908D0 (en) * | 2009-09-25 | 2009-11-11 | Molins Plc | Measurement apparatus |
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| CN108168991A (en) * | 2017-11-28 | 2018-06-15 | 昆明理工大学 | A kind of method for measuring papermaking-method reconstituted tobaccos mixture proportion in cigarette |
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