CN109444326B - A cigarette mainstream smoke main component capture detection device and analysis method - Google Patents
A cigarette mainstream smoke main component capture detection device and analysis method Download PDFInfo
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- 239000000779 smoke Substances 0.000 title claims abstract description 101
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 62
- 238000004458 analytical method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 52
- 230000000391 smoking effect Effects 0.000 claims abstract description 32
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000741 silica gel Substances 0.000 claims abstract description 19
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims description 78
- 239000003570 air Substances 0.000 claims description 60
- 238000002329 infrared spectrum Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000012080 ambient air Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000013307 optical fiber Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims 1
- 230000008569 process Effects 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 210000000214 mouth Anatomy 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 238000007405 data analysis Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013135 deep learning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001323 two-dimensional chromatography Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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Abstract
The invention discloses a main component trapping and detecting device of cigarette main stream smoke and an analysis method thereof, and aims to provide a main component trapping and detecting device of cigarette main stream smoke and an analysis method thereof, which are convenient to use. The detection device comprises a smoking machine, a bypass filter, a first electromagnetic reversing valve, a smoke storage device, a hollow waveguide fiber gas tank, an infrared spectrometer, a second electromagnetic reversing valve, a peristaltic pump and a diaphragm air pump, wherein the smoke storage device comprises a silica gel air bag, a sample inlet and a sample outlet are arranged on the silica gel air bag, a sample inlet manual switch knob and a sample outlet manual switch knob are arranged on the sample inlet, one side of the hollow waveguide fiber gas tank is provided with an air inlet, the other side of the hollow waveguide fiber gas tank is provided with an air outlet, a hollow waveguide fiber, an infrared light inlet deflection lens and an infrared light outlet deflection lens are arranged in the hollow waveguide fiber gas tank, and two ends of the hollow waveguide fiber are respectively connected with the infrared light inlet deflection lens and the infrared light outlet deflection lens.
Description
Technical Field
The invention relates to the technical field of cigarette detection equipment, in particular to a rapid and sensitive online main component trapping and detecting device for main stream smoke of cigarettes and an analysis method thereof.
Background
In the combustion process of the cigarettes, gas inhaled into the oral cavity of a consumer through the cigarette rods and the filter sticks is main stream smoke, so that the sensory experience of the consumer is directly determined by the main stream smoke, and the quality of the cigarettes is reflected. How to stably and continuously improve the quality of cigarettes is always the direction of attention and efforts in the tobacco industry. Therefore, the characteristics of the main stream smoke of the cigarettes are fully researched, so that an evaluation method of the quality of the main stream smoke is established, the sensory characteristics and the technical characteristics of the cigarette products can be more comprehensively reflected, and further the improvement of the quality improvement of the cigarette products is facilitated.
Cigarette smoke is a complex aerosol, which is mainly composed of gas, solid and steam states. In the process of researching and analyzing the components of the smoke, whether the smoke can pass through a Cambridge filter disc or not is often divided into a gas phase and a particle phase. The traditional offline mainstream smoke detection method is to extract or enrich the substances trapped in the filter disc or the filtered smoke, and analyze the substances by a chromatographic or mass spectrometry method. The detection method has complex process and long detection period, while the formation of cigarette smoke is a dynamic process, and the obtained result is only the analysis of aged smoke and partial chemical components of the disintegrated smoke after the processes of trapping, pretreatment, chromatography, mass spectrum separation and the like. Dynamic characteristics in the flue gas generation process cannot be reflected. For example, shen Qinpeng et al adopts liquid-gas chromatography to measure NNK (on-line liquid-gas two-dimensional chromatography to measure 4- (N-methylnitrosamine) -1- (2-pyridyl) -1-butanone [ J ] in main stream smoke of cigarettes with high sensitivity, 2016,44 (06): 929-934.), single detection time is 45-50 minutes, han Bing et al adopts thermal desorption-gas chromatography-mass spectrometry to enrich main stream smoke generated by burning a plurality of cigarettes, and analyzes organic compounds in the main stream smoke (thermal desorption-gas chromatography/mass spectrometry is used to analyze main gas organic compounds [ J ] of main stream smoke of cigarettes, guangdong chemical industry, 2016,43 (11): 262-264). The detection period is long, the main stream smoke of a plurality of cigarettes needs to be enriched, the quality of the cigarettes cannot be reflected from a single level, and meanwhile, the online, efficient and high-precision requirements are ensured.
The infrared spectrum (400-4000 cm < -1 >) method is an analysis method for determining the molecular structure of a substance and identifying a compound according to information such as molecular vibration, rotation and the like, has the advantages of rapidness, high sensitivity, high flux and the like, and can uniformly acquire each component of smoke and the cooperative distribution information among the components in a space-time manner. The technology is widely applied to quality analysis and evaluation in the fields of petroleum, chemical industry, food, wine and the like at present, but has few research reports on tobacco quality analysis and evaluation, and particularly lacks related reports on the application aspect of main stream smoke quality evaluation, and the main reasons are that the traditional gas infrared spectrum instrument has large dead volume and low detection sensitivity, is difficult to be seamlessly coupled with a smoking machine, and seriously hinders the application of the gas infrared spectrum technology in the tobacco industry.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an online main component trapping and detecting device for main smoke of cigarettes and an analysis method thereof, wherein the online main component trapping and detecting device has a simple structure and high detection sensitivity.
In order to solve the technical problems, the invention is realized by the following technical scheme:
The main component trapping and detecting device for the main stream smoke of the cigarettes comprises a smoking machine, a bypass filter, a first electromagnetic reversing valve, a smoke storage device, a hollow waveguide fiber gas tank, an infrared spectrometer, a second electromagnetic reversing valve, a peristaltic pump and a diaphragm air pump; the smoke storage device comprises a silica gel air bag, a sample introduction manual switch knob, a sample discharge manual switch knob, a gas inlet, a gas outlet, a hollow waveguide fiber gas tank, a hollow waveguide fiber, an infrared light inlet deflection lens and an infrared light outlet deflection lens, wherein the sample introduction manual switch knob is arranged on the sample introduction port, the sample discharge manual switch knob is arranged on the sample discharge port, the sample discharge switch knob is arranged on the sample discharge port, the gas inlet is arranged on one side of the hollow waveguide fiber gas tank, the gas outlet is arranged on the other side of the hollow waveguide fiber gas tank, a hollow waveguide fiber, the infrared light inlet deflection lens and the infrared light outlet deflection lens are arranged in the hollow waveguide fiber gas tank, two ends of the hollow waveguide fiber are respectively connected with the infrared light inlet deflection lens and the infrared light outlet deflection lens, the infrared light spectrometer comprises an infrared light incidence device and a detection device, the infrared light incidence device is used for providing incident light for the infrared light inlet deflection lens, the detection device is used for receiving infrared signals emitted by the infrared light outlet deflection lens, three ports of the first electromagnetic reversing valve are respectively connected with a smoke suction machine, a bypass filter and the sample introduction port, a first electromagnetic valve is arranged on a pipeline connecting the first electromagnetic reversing valve and the sample inlet, the sample outlet is connected with the gas inlet, a second electromagnetic valve is arranged on a pipeline connecting the sample inlet and the sample inlet, the sample discharge valve and the inlet, and the peristaltic pump is respectively connected with the three electromagnetic valves.
Preferably, the device also comprises a heating device for controlling the temperature of the hollow waveguide fiber gas tank.
Preferably, the bypass filter is a combination of an air bypass filter and an oil mist bypass filter, the filter element is made of polypropylene, the inner diameter of the filter element of the air bypass filter is 5 microns, and the filter element of the oil mist bypass filter is 0.3 microns.
An analysis method of a main component trapping and detecting device for main smoke of cigarettes, which adopts the main component trapping and detecting device for main smoke of cigarettes, comprises the following steps:
(1) Preheating and preprocessing an infrared spectrometer, namely opening a Fourier infrared spectrometer, preheating, opening a passage of a first electromagnetic reversing valve and a bypass filter, opening a first electromagnetic valve and a second electromagnetic valve, opening a passage of a second electromagnetic reversing valve and a diaphragm air pump, connecting ambient air into a bypass air inlet, opening the diaphragm air pump, sucking the ambient air or nitrogen, and evacuating residual gas in an air pipe, an air bag and a hollow waveguide optical fiber gas tank for 5 minutes;
(2) The background signal is collected, after pretreatment, the diaphragm air pump is closed, the second electromagnetic valve is closed, the standing is carried out for 30 seconds, the infrared spectrum signal at the moment is collected, and the signal is used as the background signal;
(3) The method comprises the steps of collecting and preparing smoke, namely switching a passage of a first electromagnetic reversing valve communicated with a smoking machine, cleaning gas in a silica gel gas bag through a step of cleaning the gas bag of the smoking machine, starting the smoking machine, sucking single cigarettes by the smoking machine, and collecting all smoke generated by the single cigarettes through the silica gel gas bag;
(4) Collecting spectra, namely closing a first electromagnetic valve, opening a second electromagnetic valve, switching a passage for communicating a peristaltic pump by a second electromagnetic reversing valve after the collection of the smoke is completed, setting the speed of the peristaltic pump to be 35ml/min, starting the peristaltic pump to enable the smoke in the air bag to enter a hollow waveguide fiber gas tank, measuring the infrared spectra every 30 seconds at the same time, closing the peristaltic pump after the peristaltic pump is started for 7 minutes, closing the second electromagnetic valve, enabling the smoke to stand in the hollow waveguide fiber gas tank for 5 minutes, and measuring the infrared spectra in a stable state every 30 seconds at the same time;
(5) The cleaning device is used for switching the passage from the first electromagnetic directional valve to the bypass filter, opening the first electromagnetic valve, and opening the second electromagnetic valve;
(6) And (5) data analysis.
Preferably, in the step, 7-8 cigarettes are smoked by the smoking machine, 35ml of smoke is generated in each cigarette, and the total amount of the smoke of the single cigarette is 245-280 ml.
Preferably, in the step, the hollow-core waveguide fiber gas cell has a capacity of 100ml.
Compared with the prior art, the invention has the following advantages:
(1) The smoke storage device is of a double-channel silica gel air bag structure, and the silica gel air bag is soft in material, so that the resistance of main stream smoke entering the air bag can be greatly reduced, and the smoke can be fully absorbed. The storage device has low pressure requirement on the air source, can more efficiently capture the smoke, has extremely small dead volume, is extremely favorable for rapid analysis of the main stream smoke, and improves the accuracy and repeatability of the analysis. The detection sensitivity of the invention can reach 10ppb level, and the detection is simple and quick, thereby completely meeting the analysis requirements of most trace gases.
(2) The detection device has the advantages of simple structure, wide application range, no need of pretreatment, direct-current smoke collection, and flexible and convenient use.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a detecting device according to the present invention.
Fig. 2 is a gradient infrared spectrum of a sample of smoke of an example.
Fig. 3 is an infrared spectrum of a smoke sample of the example in a steady state.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention. In the following description, for clarity of presentation of the structure and operation of the present invention, description will be made with reference to the accompanying drawings by means of various directional words, but words such as "front", "rear", "left", "right", "upper", "lower" and the like should be interpreted as words of convenience and not as limiting words.
The main component trapping and detecting device for the main stream smoke of the cigarettes comprises a smoking machine 1, a bypass filter 1.1, a first electromagnetic directional valve 2, a smoke storage device 3, a hollow waveguide fiber gas tank 4, an infrared spectrometer, a second electromagnetic directional valve 5, a peristaltic pump 6 and a diaphragm air pump 7, as shown in figure 1; the smoke storage device 3 comprises a silica gel air bag 3.1 provided with a sample inlet 3.2 and a sample outlet 3.3, a sample injection manual switch knob 3.4 arranged on the sample inlet 3.2, and a sample outlet manual switch knob 3.5 arranged on the sample outlet 3.3; an air inlet 4.2 is arranged on one side of the hollow waveguide fiber gas tank 4, an air outlet 4.3 is arranged on the other side of the hollow waveguide fiber gas tank 4, a hollow waveguide fiber 4.1, an infrared light entrance opening deflection lens 4.4 and an infrared light exit opening deflection lens 4.5 are arranged in the hollow waveguide fiber gas tank 4, two ends of the hollow waveguide fiber 4.1 are respectively connected with the infrared light entrance opening deflection lens 4.4 and the infrared light exit opening deflection lens 4.5, the infrared spectrometer comprises an infrared light incidence device 4.6 and a detection device 4.7, the infrared light incidence device 4.6 is used for providing incident light to the infrared light entrance opening deflection lens 4.4, the detection device 4.7 is used for receiving infrared signals emitted by the infrared light exit opening deflection lens 4.5, three ports of the first electromagnetic reversing valve 1 are respectively connected with a smoking machine 1, a bypass filter 1.1 and a sample inlet 3.2, a first electromagnetic valve 3.6 is arranged on a pipeline connecting the first electromagnetic reversing valve 1 and the sample inlet 3.2, the sample exit opening 3.3 is connected with the air inlet 4.2, the infrared light entrance opening 4.6 and the detection device 4.7 are respectively arranged on a pipeline connecting the first electromagnetic reversing valve 1 and the sample exit opening 3.2, and the third electromagnetic valve 3.5 are respectively arranged on the pipeline connecting the first electromagnetic reversing valve 3.2 and the second electromagnetic valve 4.5 Peristaltic pump 6 and diaphragm air pump 7 are connected.
The device also comprises a heating device (not shown in the figure) for controlling the temperature of the hollow waveguide fiber gas tank 4, wherein the heating device comprises a heat preservation device and a plurality of temperature sensors which are arranged on the pipe body, and a heating device and an embedded controller which wrap the hollow waveguide fiber gas tank. The heating device is convenient for the hollow waveguide fiber gas tank to be in a reasonable temperature area range. The heating device has an excellent heat preservation constant temperature function, can effectively reduce the heat loss of gas in a pipeline, ensures the temperature stability of the hollow waveguide fiber gas tank, and improves the analysis precision and accuracy.
The bypass filter 1.1 is a combination of an air bypass filter and an oil mist bypass filter, the filter element is made of polypropylene, the inner diameter of the filter element of the air bypass filter is 5 microns, and the filter element of the oil mist bypass filter is 0.3 microns.
An analysis method of a main component trapping and detecting device for main smoke of cigarettes, which adopts the main component trapping and detecting device for main smoke of cigarettes, comprises the following steps:
(1) The infrared spectrometer is preheated and preprocessed, namely, a Fourier infrared spectrometer is opened and preheated, a passage between a first electromagnetic reversing valve 2 and a bypass filter 1.1 is opened, a first electromagnetic valve 3.6 and a second electromagnetic valve 3.7 are opened, a passage between a second electromagnetic reversing valve 5 and a diaphragm air pump 7 is opened, ambient air is connected to a bypass air inlet, the diaphragm air pump 7 is opened, ambient air or nitrogen is sucked, and residual gas in an air pipe, an air bag and a hollow waveguide fiber gas tank is exhausted for 5 minutes;
(2) The background signal is collected, after pretreatment, the diaphragm air pump is closed, the second electromagnetic valve is closed for 3.7, and the standing is carried out for 30 seconds, the infrared spectrum signal at the moment is collected, and the signal is taken as the background signal;
(3) The method comprises the steps of collecting and preparing smoke, namely switching a passage of a first electromagnetic directional valve 2 communicated with a smoking machine 1, cleaning gas in a silica gel gas bag 3.1 through a gas bag cleaning step of the smoking machine, starting the smoking machine, sucking single cigarettes through the silica gel gas bag, collecting all smoke generated by the single cigarettes through the silica gel gas bag, sucking 7-8 cigarettes through the smoking machine, generating 35ml of smoke per mouth, wherein the total amount of all smoke of the single cigarettes is 245ml-280ml, and adopting an RM1/PULS single-pore-channel smoking machine (Germany Borgwaldt KC company);
(4) Collecting spectra, namely closing a first electromagnetic valve 3.6, opening a second electromagnetic valve 3.7, switching a passage for communicating a second electromagnetic reversing valve 5 with a peristaltic pump 6 after the collection of the smoke is completed, setting the speed of the peristaltic pump to be 35ml/min, starting the peristaltic pump to enable the smoke in the air bag to enter a hollow waveguide fiber gas tank, wherein the capacity of the hollow waveguide fiber gas tank is 100ml, measuring the infrared spectra every 30 seconds at the same time, closing the peristaltic pump 5 after the peristaltic pump is started for 7 minutes, closing the second electromagnetic valve 3.7, enabling the smoke to stand in the hollow waveguide fiber gas tank for 5 minutes, and measuring the infrared spectra in a stable state every 30 seconds while standing;
(5) The cleaning device comprises a first electromagnetic directional valve 2, a second electromagnetic valve 3.7, a diaphragm air pump 7, a cleaning pipeline, a silica gel air bag and residual flue gas in a hollow waveguide fiber gas tank, wherein the first electromagnetic directional valve 2 is switched to a bypass filter 1.1;
(6) And (5) data analysis.
During analysis, the first electromagnetic reversing valve, the second electromagnetic reversing valve, the first electromagnetic valve, the second electromagnetic valve, the peristaltic pump and the diaphragm air pump are controlled by an embedded controller.
Examples
Experimental materials are classical cigarette of Hongtaishan, yuxi hard harmonious cigarette;
the above test materials were used for analysis as follows:
(1) The infrared spectrometer is preheated and preprocessed, namely, a Fourier infrared spectrometer is opened and preheated, a passage between a first electromagnetic reversing valve 2 and a bypass filter 1.1 is opened, a first electromagnetic valve 3.6 and a second electromagnetic valve 3.7 are opened, a passage between a second electromagnetic reversing valve 5 and a diaphragm air pump 7 is opened, ambient air is connected to a bypass air inlet, the diaphragm air pump 7 is opened, ambient air or nitrogen is sucked, and residual gas in an air pipe, an air bag and a hollow waveguide fiber gas tank is exhausted for 5 minutes;
(2) The background signal is collected, after pretreatment, the diaphragm air pump is closed, the second electromagnetic valve is closed for 3.7, and the standing is carried out for 30 seconds, the infrared spectrum signal at the moment is collected, and the signal is taken as the background signal;
(3) The method comprises the steps of collecting and preparing smoke, namely switching a passage of a first electromagnetic directional valve 2 communicated with a smoking machine 1, cleaning gas in a silica gel gas bag 3.1 through a gas bag cleaning step of the smoking machine, starting the smoking machine and sucking single cigarettes (classical red tower mountain cigarettes, yuxi hard and Harmonious cigarettes) through the smoking machine, collecting all the smoke generated by the single cigarettes through the silica gel gas bag, sucking 7-8 cigarettes by the smoking machine, generating 35ml of smoke at each mouth, wherein the total amount of all the smoke of the single cigarettes is 245ml-280ml, and adopting an RM1/PULS single-pore-channel smoking machine (Germany Borgwaldt KC company) by the smoking machine;
(4) Collecting spectra, namely after the collection of the smoke is completed, closing a first electromagnetic valve 3.6, opening a second electromagnetic valve 3.7, switching a passage of the second electromagnetic reversing valve 5 communicated with a peristaltic pump 6, setting the speed of the peristaltic pump to be 35ml/min, starting the peristaltic pump to enable the smoke in the air bag to enter a hollow waveguide fiber gas tank, wherein the capacity of the hollow waveguide fiber gas tank is 100ml, measuring an infrared spectrum every 30 seconds to obtain a smoke gradient infrared spectrum shown in figure 2, closing the peristaltic pump 5 after the peristaltic pump is started for 7 minutes, closing the second electromagnetic valve 3.7, enabling the smoke to stand in the hollow waveguide fiber gas tank for 5 minutes, and measuring the infrared spectrum in a stable state every 30 seconds while standing to obtain a stable smoke infrared spectrum shown in figure 3;
(5) The cleaning device comprises a first electromagnetic directional valve 2, a second electromagnetic valve 3.7, a diaphragm air pump 7, a cleaning pipeline, a silica gel air bag and residual flue gas in a hollow waveguide fiber gas tank, wherein the first electromagnetic directional valve 2 is switched to a bypass filter 1.1;
(6) Data analysis fig. 2 is an infrared spectrum collected during the flue gas sample injection process, and as can be seen from fig. 2, the infrared spectrum of trace flue gas at the beginning of sample injection can be measured, and meanwhile, the infrared spectrum which changes in gradient along with the linear increase of flue gas volume can be observed, so that the method has the characteristics of high sensitivity and quick response. Fig. 3 is an infrared spectrum chart in a stable state after the smoke sample injection is completed, and as can be seen from fig. 3, the detection method of the invention has good reproducibility on infrared spectrum information of main stream smoke, and can accurately capture main hazard component information in the main stream smoke, such as carbon monoxide, hydrocyanic acid, ammonia and the like.
The invention adopts the national standard method to collect main stream smoke, so that each mouth of the smoking machine can smoke for 2 seconds, 35ml of main stream smoke is generated at each mouth, and the interval between two times of smoking is 1 minute. The single cigarette is about 7-8 in need of completing smoking, and the 7-8 smoke of the single cigarette is uniformly mixed in advance, so that the mutation of the components of the single mainstream smoke is effectively avoided, the accuracy and the stability of the subsequent online spectral analysis are ensured, and the stability of the components of the mainstream smoke is further improved. The invention adopts the quantifiable peristaltic pump, and the flow rate of the peristaltic pump is set at 35ml/min, so that the smoke continuously and stably enters the hollow waveguide fiber gas tank, and the influence of unstable flow of the gas on the detection result is avoided.
The inner wall of the hollow waveguide fiber in the hollow waveguide fiber gas tank is an Ag/AgI film layer, so that signals with the wavelength of 2-20 microns can be filtered out, and the efficiency is enhanced. Meanwhile, incident light can be reflected in the hollow waveguide fiber gas tank for multiple times, so that the contact frequency with the gas to be detected is increased, the absorption intensity of the gas to be detected in a middle infrared band is improved, and the sensitivity and the accuracy of the system are further improved. Under the accumulation of a large amount of spectrum data, the analysis chemistry technology and the deep learning method are applied to accurately extract the characteristics and the content of main components in the main stream smoke of cigarettes from the spectrum data, and a characteristic library of the main stream smoke of cigarettes of different types is constructed. Realizes the online real-time detection of the main stream smoke of the cigarettes, and is a simple, convenient, quick and sensitive main stream smoke instrument analysis method.
The method can comprehensively analyze the components of the main stream smoke generated after the cigarette is smoked and combusted, has accurate and rapid identification process and high sensitivity, is not only suitable for detecting the components of the combustion smoke in the cigarette industry, but also is expected to meet the evaluation requirement of the quality of the main stream smoke of the cigarette product, and improves the technical support for the subsequent formula design and process quality control.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (4)
1. The analysis method of the main component trapping and detecting device for the main smoke of the cigarettes is characterized by adopting the main component trapping and detecting device for the main component of the main smoke of the cigarettes, and comprises a smoking machine (1), a bypass filter (1.1), a first electromagnetic reversing valve (2), a smoke storage device (3), a hollow waveguide fiber gas tank (4), an infrared spectrometer, a second electromagnetic reversing valve (5), a peristaltic pump (6) and a diaphragm air pump (7), wherein the smoke storage device (3) comprises a silica gel air bag (3.1) provided with a sample inlet (3.2) and a sample outlet (3.3), a sample injection manual switch knob (3.4) arranged on the sample inlet (3.2), and a sample outlet manual switch knob (3.5) arranged on the sample outlet (3.3), one side of the hollow waveguide fiber gas tank (4) is provided with an air inlet (4.2), the other side of the hollow waveguide fiber gas tank is provided with an air outlet (4.3), and the hollow waveguide fiber gas tank (4) is internally provided with a hollow waveguide fiber (4.1) The infrared spectrometer comprises an infrared light incidence device (4.6) and a detection device (4.7), wherein the infrared light incidence device (4.6) is used for providing incident light to the infrared light incidence port deflection lens (4.4), the detection device (4.7) is used for receiving infrared signals emitted by the infrared light emission port deflection lens (4.5), three ports of the first electromagnetic reversing valve (2) are respectively connected with a smoking machine (1), a bypass filter (1.1) and a sample inlet (3.2), a first electromagnetic valve (3.6) is arranged on a pipeline connecting the first electromagnetic reversing valve (2) and the sample inlet (3.2), the sample outlet (3.3) is connected with an air inlet (4.2), and peristaltic pumps (3.7) are respectively arranged on the three ports of the first electromagnetic reversing valve (2) and the air inlet (3.2);
the analysis method comprises the following steps:
(1) Preheating and preprocessing an infrared spectrometer, namely opening a Fourier infrared spectrometer and preheating, opening a passage between a first electromagnetic directional valve (2) and a bypass filter (1.1), opening a first electromagnetic valve (3.6) and a second electromagnetic valve (3.7), opening a passage between a second electromagnetic directional valve (5) and a diaphragm air pump (7), accessing ambient air at a bypass air inlet, opening the diaphragm air pump (7), sucking the ambient air or nitrogen, and exhausting residual gas in an air pipe, an air bag and a hollow waveguide optical fiber gas tank for 5 minutes;
(2) The background signal is collected, after pretreatment, a diaphragm air pump is closed, a second electromagnetic valve (3.7) is closed, standing is carried out for 30 seconds, an infrared spectrum signal at the moment is collected, and the signal is used as a background signal;
(3) The method comprises the steps of collecting and preparing smoke, namely switching a passage of a first electromagnetic reversing valve (2) communicated with a smoking machine (1), cleaning gas in a silica gel gas bag (3.1) through a gas bag cleaning step of the smoking machine, starting the smoking machine, sucking single cigarettes by the smoking machine, and collecting all smoke generated by the single cigarettes through the silica gel gas bag;
(4) Collecting spectra, namely closing a first electromagnetic valve (3.6) after the collection of the smoke is completed, opening a second electromagnetic valve (3.7), switching a passage for connecting a second electromagnetic reversing valve (5) with a peristaltic pump (6), setting the speed of the peristaltic pump to be 35ml/min, starting the peristaltic pump to enable the smoke in the air bag to enter a hollow waveguide fiber gas tank, measuring the infrared spectra every 30 seconds at the same time, closing the peristaltic pump (6) after the peristaltic pump is started for 7 minutes, closing the second electromagnetic valve (3.7), enabling the smoke to stand in the hollow waveguide fiber gas tank for 5 minutes, and measuring the infrared spectra in a stable state every 30 seconds at the same time of standing;
(5) The cleaning device comprises a first electromagnetic directional valve (2) and a bypass filter (1.1), a first electromagnetic valve (3.6) and a second electromagnetic valve (3.7) which are switched, a diaphragm air pump (7) and a pipeline, a silica gel air bag and residual smoke in a hollow waveguide fiber air tank which are cleaned, wherein the pipeline is opened by switching the first electromagnetic directional valve (2);
(6) Analyzing data;
In the step (3), 7-8 cigarettes are required to be smoked by the smoking machine, 35ml of smoke is generated in each cigarette, and the total amount of the whole smoke of the single cigarette is 245-280 ml.
2. The analysis method of the main component trapping and detecting device for main stream smoke of cigarettes according to claim 1, further comprising a heating device for controlling the temperature of the hollow waveguide fiber gas tank (4).
3. The method for analyzing the main component trapping and detecting device for the main stream smoke of the cigarettes according to claim 1, wherein the bypass filter (1.1) is a combination of an air bypass filter and an oil mist bypass filter, the filter element is made of polypropylene, the inner diameter of the filter element of the air bypass filter is 5 microns, and the filter element of the oil mist bypass filter is 0.3 microns.
4. The method for analyzing main constituents of mainstream smoke of a cigarette according to claim 1, wherein the hollow waveguide fiber gas cell has a capacity of 100ml in the step (4).
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| CN110274886A (en) * | 2019-06-13 | 2019-09-24 | 广东化一环境科技有限公司 | A kind of oil smoke on-line measuring device and method |
| CN110779950B (en) * | 2019-10-22 | 2024-12-03 | 云南巴菰生物科技股份有限公司 | A smoke output detector for heat-not-burn cigarettes |
| CN112362416A (en) * | 2020-11-19 | 2021-02-12 | 西安热工研究院有限公司 | Air bag sampling intermittent type flue gas measuring system |
| CN112881323B (en) * | 2021-01-14 | 2022-03-08 | 云南中烟工业有限责任公司 | Quality evaluation method of cigarette mainstream smoke |
| CN112666086A (en) * | 2021-01-14 | 2021-04-16 | 云南中烟工业有限责任公司 | Coupling method of hollow waveguide infrared spectrometer and smoking machine |
| CN112749906B (en) | 2021-01-14 | 2024-09-20 | 云南中烟工业有限责任公司 | Sensory evaluation method for spectral data of main stream smoke of cigarettes |
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