CN115248229B - A method for studying the adsorption amount of atomizer in tobacco - Google Patents
A method for studying the adsorption amount of atomizer in tobacco Download PDFInfo
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- CN115248229B CN115248229B CN202110465905.6A CN202110465905A CN115248229B CN 115248229 B CN115248229 B CN 115248229B CN 202110465905 A CN202110465905 A CN 202110465905A CN 115248229 B CN115248229 B CN 115248229B
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Abstract
本发明提供一种烟草中雾化剂吸附量的研究方法，包括：选取待测烟草，利用化学吸附仪向所述待测烟草中通入雾化剂使其吸附饱和，应用程序升温脱附技术测定所述待测烟草中雾化剂的脱附结果。本发明的烟草中雾化剂吸附量的研究方法，应用程序升温脱附技术，以测定雾化剂在烟草表面吸脱附的角度，通过探究雾化剂在烟草表面的吸脱附性能，来获得更多关于雾化剂与烟草之间相互作用的信息。
The present invention provides a method for studying the adsorption amount of an atomizer in tobacco, comprising: selecting tobacco to be tested, introducing an atomizer into the tobacco to be tested using a chemical adsorption instrument to make it adsorbed saturated, and applying an application temperature rise desorption technique to determine the desorption result of the atomizer in the tobacco to be tested. The method for studying the adsorption amount of an atomizer in tobacco of the present invention uses an application temperature rise desorption technique to determine the adsorption and desorption angles of the atomizer on the tobacco surface, and by exploring the adsorption and desorption performance of the atomizer on the tobacco surface, more information about the interaction between the atomizer and the tobacco is obtained.
Description
Technical Field
The invention relates to the field of tobacco, in particular to a research method for the adsorption quantity of an atomizing agent in tobacco.
Background
The moisture content of the tobacco raw material is an important index for influencing the sensory comfort, the atomizing agent is a substance with strong capability of absorbing moisture from the environment and keeping the moisture, and the polyol compound such as glycerol is the most widely used atomizing agent in the tobacco industry at present. Researches show that the polyalcohol compounds such as glycerin and the like can be transferred into smoke in the smoking process of cigarettes/heated cigarettes, are positively correlated with the release amount of the smoke, and can be cracked to generate carbonyl compounds such as formaldehyde, acetaldehyde, propionaldehyde, acrolein, crotonaldehyde and the like, and the carbonyl compounds can stimulate respiratory systems and sense organs of human bodies to different degrees.
Current studies on the content of the atomizing agent in the tobacco mainly determine the percentage of the atomizing agent in the tobacco by measuring the mass of the tobacco and adding the mass of the atomizing agent, and determine the optimal adding amount of the atomizing agent by trying not to pass through the percentage content of the atomizing agent. The method for researching the content of the atomizing agent still belongs to macroscopic research, and the capability of the tobacco for attaching the content of the atomizing agent cannot be explored from a more microscopic angle, and further data information cannot be obtained, so that the deep research and development of the atomizing agent in the tobacco are hindered.
Disclosure of Invention
The invention provides a research method of the adsorption quantity of an atomizing agent in tobacco, which is used for solving the technical problems.
The invention provides a research method for the adsorption quantity of an atomizing agent in tobacco, which comprises the steps of selecting tobacco to be detected, introducing the atomizing agent into the tobacco to be detected by using a chemical adsorption instrument to enable the tobacco to be detected to be adsorbed and saturated, and measuring the desorption result of the atomizing agent in the tobacco to be detected by using a temperature programming desorption technology.
The invention provides a research method for the first time, a temperature programming desorption technology is applied to determine the desorption angle of the atomizing agent on the tobacco surface, and more information about interaction between the atomizing agent and the tobacco is obtained by exploring the adsorption and desorption performance of the atomizing agent on the tobacco surface. The atomizing agent may be, for example, a polyol compound such as glycerin.
The temperature programmed desorption is a method for heating the adsorbent with adsorbed adsorbate according to a preset temperature program (such as constant temperature rise) to obtain a desorption amount and temperature relation diagram of the adsorbate. The invention utilizes a chemical adsorption instrument and applies a temperature programming desorption technology, can in-situ examine the reaction condition of adsorption molecule atomizing agent and the tobacco solid surface, and can provide a plurality of information about the tobacco surface result. The temperature programmed desorption technology is very sensitive to physical parameters of the surface of the adsorbate, has high identification capability, and can be used for researching the nature of the surface of the tobacco carrier and the effect of different atomizing agents or the nature of the surface of different tobacco carriers and the effect of atomization.
The invention establishes the saturated adsorption quantity and desorption quantity of the atomizing agent in the tobacco raw material by using the temperature programming desorption method, and the detection method of the desorption temperature of the atomizing agent, and the detection is rapid. The experimental result obtained by the temperature programming desorption method can be used for knowing the influence factors of the saturated adsorption quantity of the atomizing agent, providing reference for controlling the content of the atomizing agent in the tobacco raw material, and providing more dimensional information and directions for research and development of the tobacco and the atomizing agent.
For example, the current direction of improvement of tobacco and aerosol is mainly focused on the macroscopic level, and the preferred percentage of aerosol is generally adjusted by observing the moisture absorption and smoke generation of tobacco only by taking different amounts of aerosol. The effect of the surface properties, as well as the atomizer properties on the amount added is not known for the adsorption capacity of tobacco. The interaction between the atomizing agent and the tobacco surface is known by adopting the temperature programming desorption analysis technology, so that the influence of the surface condition of the tobacco on the adsorption of the atomizing agent can be explored, and data support is provided for the research directions of the pore size, specific surface area, surface modification and the like of the tobacco surface. In addition, the adsorption rule of the tobacco sheet prepared from different process materials on the atomizing agent (such as the polyalcohol compound such as glycerol) can be clarified.
Further, the adsorption rule of the tobacco to be detected is deduced according to the desorption result. The invention relates to a research method for the adsorption quantity of an atomizing agent in tobacco, which can carry out desorption measurement after the adsorption saturation of the atomizing agent, so as to obtain a desorption curve of the atomizing agent in tobacco, and understand the desorption rule of the atomizing agent.
The chemical adsorption instrument used for the programmed temperature desorption of the invention can be a chemical adsorption instrument commonly used at present, such as a microphone adsorption instrument and the like.
Further, when the adsorption and desorption measurement is performed on the tobacco to be tested, the tobacco to be tested is pretreated, namely, the impurities on the surface of the tobacco are removed first. The method comprises the steps of adding tobacco to be detected into a chemical adsorption instrument, introducing inert gas into the tobacco to be detected in the chemical adsorption instrument, and heating, so that impurities adsorbed on the surface of the tobacco to be detected are removed by heating and introducing the inert gas. And then taking inert gas as carrier gas, taking the carrier gas carrying the atomizing agent as pretreatment gas, and introducing pretreatment gas into the tobacco to be tested. Specifically, the chemical adsorption instrument comprises a Loop sampling tube, the pretreatment device is introduced into tobacco to be detected after passing through the Loop sampling tube in the chemical adsorption instrument, and the tobacco to be detected adsorbs an atomizing agent in pretreatment gas until adsorption is saturated. And then starting temperature programming, and performing desorption test. In the temperature programming desorption technology, the carrier gas can pass through a U-shaped quartz tube for placing tobacco, and the carrier gas continuously circulates to carry away the atomized agent volatilized by heating in the tube.
The pretreatment step of the invention comprises impurity removal and adsorption processes, wherein inert gas is introduced into the tobacco to be detected during impurity removal, and inert gas and an atomizing agent are introduced into the tobacco to be detected after a period of time for adsorption, so that the tobacco to be detected adsorbs the atomizing agent to be saturated, and then the subsequent temperature programming desorption is performed. The time of the whole pretreatment step including the impurity removal and the adsorption of the present invention is 25 to 40min, preferably 30min, and the heating is performed during the whole pretreatment step at 140 to 160 ℃, preferably 150 ℃.
The Loop sample feeding tube in the chemical adsorption instrument is called an annular quantitative sample feeding tube, and the volume of the pretreatment gas of each needle is fixed due to the fixed volume.
The inventor finds that the volume of gas entering the tobacco to be detected through the Loop sample injection pipe is fixed when each sample is injected because the volume of the Loop sample injection pipe in the chemical adsorption instrument is fixed. And, the content of the atomizing agent carried in the carrier gas is fixed, so that the content of the atomizing agent which is introduced into the thermal conductivity detector during each sample injection is fixed. It is known that the content of the atomizing agent at each sample injection depends on the volume of the Loop sample injection tube. The existing Loop sampling tube has a large volume of 5.0cm 3, so that sampling saturation is achieved by sampling for a small number of times (1-2 times) in the actual measurement process, accuracy and sensitivity are reduced, and a large error is generated in the measurement result.
The inventor finds that the volume modification of the Loop sample injection pipe to be 0.5-1cm 3 is more suitable for measuring the desorption amount of the tobacco surface atomizer through research tests. Specifically, loop sampling pipes with proper volumes can be selected according to the content of the atomizing agents of different novel tobaccos. The method can be used for measuring the content of the atomizing agent reaching adsorption saturation on the surface of the tobacco product material on the premise of keeping accuracy and sensitivity, and can be used for measuring the saturated adsorption quantity of different tobacco raw material materials to the atomizing agent quickly by realizing Loop sampling for more than 5-10 times.
Furthermore, as the Loop sample feeding pipe is wound on the cylindrical structure in the chemical adsorption instrument, the two ends of the sample feeding pipe are communicated with the sample feeding valve, and the volume of the Loop sample feeding pipe can be reduced by shortening the length of the Loop sample feeding pipe, so that the Loop sample feeding pipe is refitted into 0.5-1cm 3. The Loop sample injection pipe is modified in a mode of shortening the length of the Loop sample injection pipe, other structures in the chemical adsorption instrument can be not required to be changed, the length of the Loop sample injection pipe is reduced, namely, the number of turns wound on the cylindrical structure is reduced, and the modification is convenient.
The method for researching the adsorption quantity of the atomizing agent in the tobacco comprises the following steps of adding the tobacco to be detected into a chemical adsorption instrument, heating, introducing inert gas into the tobacco to be detected for impurity removal, taking the inert gas as carrier gas, taking the atomizing agent carried by the carrier gas as pretreatment gas, introducing the pretreatment gas into the tobacco to be detected through a Loop sampling tube in the chemical adsorption instrument, so that the tobacco to be detected reaches adsorption equilibrium, and carrying out desorption treatment, namely carrying out desorption treatment on the tobacco to be detected after adsorption under the atmosphere of the inert gas, and obtaining a desorption curve of the tobacco to be detected. For example, in the temperature programmed desorption technique, the carrier gas passes through a U-shaped quartz tube in which the tobacco is placed, and the carrier gas continuously circulates to carry away the heated and volatilized aerosol in the tube.
Further, the pretreatment temperature is 145-155 ℃, preferably 150 ℃, and the pretreatment time is 25-35min, preferably 30min.
Further, the temperature of the desorption treatment is 180-250 ℃, preferably 200 ℃, and the time of the desorption treatment is 90-150min.
According to the method, the saturated adsorption quantity of the atomizing agent on the tobacco to be detected is calculated according to the adsorption balance of the tobacco to be detected, and after the saturated adsorption quantity is obtained, a desorption test can be performed to obtain a desorption curve.
Further, the inert gas (i.e., carrier gas) may be selected from nitrogen or helium.
Drawings
FIG. 1 shows a schematic diagram of a chemisorber in accordance with an embodiment of the invention;
FIG. 2 shows a schematic diagram of a Loop feed tube modification in accordance with an embodiment of the present invention;
FIG. 3 shows a Loop feed tube connection schematic diagram in accordance with an embodiment of the present invention;
fig. 4 shows a time-dependent desorption glycerin curve of the monoclinic tobacco sample obtained in example 1 during temperature programmed desorption;
Fig. 5 shows the time-dependent desorption glycerin curve of the monoclinic tobacco sample obtained in example 2 during the temperature-programmed desorption.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present invention with specific examples. While the description of the invention will be described in connection with the preferred embodiments, it is not intended to limit the inventive features to the implementation. Rather, the purpose of the invention described in connection with the embodiments is to cover other alternatives or modifications, which may be extended by the claims based on the invention. The following description contains many specific details for the purpose of providing a thorough understanding of the present invention. The invention may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The terms "first," "second," and the like are used merely to distinguish between descriptions and are not to be construed as indicating or implying relative importance.
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
Fig. 1 shows a schematic diagram of a chemisorber and fig. 2 shows a Loop feed tube modification schematic. In connection with fig. 1 and 2, the process gas in fig. 1 is the gas entering the reaction tube during the pretreatment, which is the inert gas, in the pretreatment step, and is used for removing impurities in the pretreatment step. The invention can be used without cold trap or cold trap. The cold trap has the function that in the impurity removal step, inert gas can bring out impurities in tobacco after passing through the tobacco to be detected, and then the impurities can be adsorbed through the cold trap. In the adsorption process in pretreatment, carrier gas and an atomizer are fed into tobacco to be detected together through a six-way valve by pulse gas, the process of adsorbing the atomizer by the tobacco is carried out, and the subsequent programmed temperature desorption test is carried out after adsorption saturation.
In the desorption treatment step, the pulse gas is a gas such as helium that brings an atomizing agent volatilized at a high temperature in a reaction tube heated in a high-temperature furnace into a Loop feed tube. And when the sample injection operation is carried out, the Loop sample injection pipe is connected with the six-way valve, wherein the pulse gas inlet is communicated with the reaction gas inlet, one end of the Loop sample injection pipe is communicated with the pulse gas inlet, and the other end of the Loop sample injection pipe is communicated with the reaction gas inlet. The high-temperature volatilized atomizing agent in the reaction tube is injected into the Loop ring through the pulse air inlet, after the Loop ring is filled, the Loop ring is communicated with the reaction air inlet, and the volatilized atomizing agent is pushed by the reaction gas conveyed by the pipeline to enter the thermal conductivity detector (TCD detector) for analysis.
The reaction gas is the gas entering the reaction tube during desorption, such as helium. In other embodiments, other gases capable of undergoing chemical reactions may be employed as the reactant gases to explore other properties of the tobacco in the reactor tube for subsequent further research.
FIG. 3 shows a Loop sample tube connection schematic. The Loop sampling tube is wound on the cylindrical structure, and two ends extending out after winding are respectively connected to the sampling valve through fixing nuts. The annular shell is sleeved on the periphery of the cylindrical structure and is fixed through an annular nut. The Loop sampling tube of the embodiment is arranged in a valve cover at the top of the chemical adsorption instrument, is fixed on a mounting plate by a ring nut, the periphery of the Loop is protected by a ring-shaped shell, and two ends of the ring are connected with a sampling valve with temperature control. The Loop sampling pipe can be replaced according to the adsorption quantity. For example, the Loop sampling pipe with the length reduced can be replaced, and the specific operation modes are as follows:
1) The temperature of the instrument is confirmed to be at the room temperature, the temperature of the heating belt can be set to be at the room temperature by a manual control mode, and the instrument is waited for cooling down.
2) The screw of the upper cover of the chemical adsorption instrument is unscrewed, the upper cover is removed, and the front cover can be pulled forward.
3) The two fixing bolts of the valve cover are pulled out, and the valve cover can be moved away by lifting the valve cover upwards.
4) The valve insulation spacer is removed.
5) The ring nut is unscrewed, the ring shell is taken down, and the middle screw of the Loop sampling tube is unscrewed, so that the Loop sampling tube can be taken down.
6) And unscrewing the clamping sleeve at the head of the Loop sampling tube by using a spanner.
7) The Loop sampling tube is lifted upwards, and can be taken down from the mounting plate.
8) And installing a new Loop sampling tube, connecting two ends of the sampling tube with a sampling valve, and screwing the annular shell 2 with fingers.
9) The Loop sample tube is pressed into place so as to be contacted with the mounting plate.
10 Tightening the Loop sampling tube fixing screw.
11 Screw on the shell is screwed down to fix the new Loop sampling tube.
12 The insulating spacer is well installed again, and the valve cover is well installed again.
13 Push up the front panel of the chemical adsorption instrument and cover the upper cover.
14 After the ring is assembled, the Loop sampling tube is corrected again, and the actual volume of the new Loop sampling tube is determined.
Example 1
Taking a monoclinic tobacco (Hunan C picked) sample as tobacco to be tested, removing impurities of the sample under the atmosphere of 100 ℃ C, N 2, then introducing glycerin for adsorption, naturally cooling to 30 ℃ in a sample tube for 30min in the whole pretreatment process, then heating to 200 ℃ at the temperature rising rate of 10 ℃ per min under the atmosphere of N 2, and keeping the temperature of the sample at 200 ℃ for 90min. As can be seen from fig. 4, the glycerin on the surface of the material starts to be desorbed significantly at 200 ℃, and a significant desorption peak appears when it is desorbed for 90min at 200 ℃.
It was found from example 1 that a significant desorption peak occurred at 200 ℃ for 90min, but the peak of TCD signal of the glycerol thermal conductivity detector was weak at this time, so that it was necessary to extend the desorption time to continue the measurement. In addition, glycerol is highly viscous and the desorbed glycerol is highly adsorbed in the tubing of the instrument, thus requiring an increase in pretreatment temperature.
Example 2
Still taking a monoclinic tobacco sample as an example, the pretreatment and desorption method is the same as in example 1, except that the temperature of the pretreatment is raised to 150 ℃, and the pretreatment is maintained for 120min after the temperature is raised to 200 ℃ in the desorption test.
As can be seen from FIG. 5, the first desorption peak starts to appear when the temperature of the sample is programmed to 180 ℃, the peak is completed in 20min, the second desorption peak appears in 40-60min, the peak is completed in 100min, and the third desorption peak appears in 100-140 min. The three adsorption modes of the glycerin adsorption on the surface of the sample are shown, the first two glycerin desorption peaks are physical adsorption of glycerin on the surface of the sample, and the third desorption peak corresponds to chemical adsorption of glycerin.
According to the above embodiment, it can be found that by performing a chemical adsorption and desorption measurement on a tobacco sample, various information can be obtained, and the specific effects are as follows:
(1) And (3) measuring saturated adsorption amounts of different tobacco raw material sheets on the polyol compounds such as glycerol through the modified chemical adsorption instrument, judging when adsorption reaches equilibrium, and calculating the saturated adsorption amounts of the polyol compounds such as glycerol of different tobacco raw material sheets through data fitting treatment.
(2) And measuring and calculating the adsorption and desorption balance of different tobacco raw material sheets on the polyol compounds such as glycerol by using the modified chemical adsorption instrument, and measuring the adsorption quantity of the polyol compounds such as glycerol on the tobacco raw material under the condition of normal temperature and normal pressure.
(3) The change in the desorption amount of the polyol compound such as glycerin adsorbed on the surface of the tobacco product material during the temperature programming at 30 ℃ and 350 ℃ was measured by the modified chemical adsorption instrument. Judging the adsorption strength of the polyol compounds such as glycerol on the surface of the tobacco material, and analyzing the correlation between the adsorption and desorption of the polyol compounds such as glycerol on the surface of the tobacco material.
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing is a further detailed description of the invention with reference to specific embodiments, and it is not intended to limit the practice of the invention to those descriptions. Various changes in form and detail may be made therein by those skilled in the art, including a few simple inferences or alternatives, without departing from the spirit and scope of the present invention.
Claims (5)
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| CN102128763B (en) * | 2010-11-16 | 2012-07-04 | 上海烟草集团有限责任公司 | Method for testing humid keeping performance of tobacco |
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