CN111366661B - Cigarette smoke extraction device and method - Google Patents
Cigarette smoke extraction device and method Download PDFInfo
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- CN111366661B CN111366661B CN201811603011.3A CN201811603011A CN111366661B CN 111366661 B CN111366661 B CN 111366661B CN 201811603011 A CN201811603011 A CN 201811603011A CN 111366661 B CN111366661 B CN 111366661B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention provides a cigarette smoke extraction device, which comprises a smoke catcher, a separation structure, a closed container and a power device, wherein the smoke catcher is connected with the separation structure; the smoke catcher is arranged in the closed container; the separation structure is used for separating the flue gas catcher; the power device is used for driving the extraction solution to flow in the closed container. The invention also provides a cigarette smoke extraction method, which comprises the following steps of 1: smoking cigarettes by using a smoking machine, and trapping smoke particulate matters of the cigarettes by using a smoke catcher; step 2: extracting the particulate matters in the cigarette smoke by using a cigarette smoke extraction device; and step 3: the extraction solution was subjected to gas chromatography analysis. The invention provides a cigarette smoke extraction device and method, which solve the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
Description
Technical Field
The invention relates to the technical field of detection of cigarette smoke components, in particular to a cigarette smoke extraction device and a method.
Background
The cigarette smoke is a complex mixed system formed by a series of chemical reactions of gasifying, decomposing, dehydrating, aromatizing, oxidizing, reducing and the like of chemical components in tobacco under the combustion condition or gasifying, condensing and the like at a certain temperature. The mainstream smoke generally consists of a particulate phase and a gas phase, wherein the particulate phase components of the cigarette smoke are usually collected by a smoke collector for analysis, and then a glass fiber filter disc is taken out from the smoke collector and placed in an extraction bottle for solvent extraction.
The calculation method of the Total Particulate Matter (TPM) is the weight difference of the smoke catcher before and after pumping, and the determination method of the chemical components in the total particulate matter is the method of taking out a glass fiber filter and adding a solvent for extraction. However, the particle phase matter contains part of volatile components, and the problems of loss of the volatile components and residue of the trap exist in the process of opening the smoke trap and taking out the glass fiber filter disc. Taking a cigarette which is not combusted by heating as an example, the moisture accounts for more than 70% of the total particulate matter, and serious moisture loss and moisture residue exist in the process of taking out the glass fiber filter disc, so that the moisture measurement result is low, and further, the calculated NFDPM (nicotine and moisture subtracted from the total particulate matter) value is high, and the NFDPM value is called as tar in the traditional cigarette. The traditional method for measuring the aroma components needs to concentrate the extract liquid by nitrogen blowing or rotary evaporation and the like, so that the operation is troublesome and the low-boiling-point aroma components are easy to lose.
Therefore, the technical problems to be solved urgently by the technical personnel in the field are that the existing cigarette smoke measuring method has inaccurate measuring result and complicated operation steps.
Disclosure of Invention
In view of the above, the invention provides a cigarette smoke extraction device and method, which solve the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
The invention provides a cigarette smoke extraction device which comprises a smoke catcher, a separation structure, a closed container and a power device.
The smoke catcher is arranged in the closed container;
preferably, the separation structure comprises a fixed structure and a moving structure, the fixed structure is used for fixing the smoke catcher, and the moving structure separates the smoke catcher;
the fixed structure is used for fixing the rear part of the smoke catcher;
the motion structure is used for separating the front part of the smoke trap in the closed container from the rear part of the smoke trap;
the power device is used for driving the extraction solution to flow in the closed container.
Preferably, the moving structure comprises a first electromagnetic generating component and a first motor, the fixed structure comprises a second electromagnetic generating component, and the front part and the rear part of the smoke catcher are both provided with a first electromagnetic adsorbing component;
the first motor drives the first electromagnetic generating component to move to the first electromagnetic absorption component, so that the first electromagnetic generating component is magnetically connected with the first electromagnetic absorption component.
More preferably, the moving structure further includes a separating rod, one end of the separating rod is provided with a first electromagnetic generating component, and the first motor drives the first electromagnetic generating component to move to the first electromagnetic adsorbing component, so that the first electromagnetic generating component is magnetically connected with the first electromagnetic adsorbing component.
The first electromagnetic generating component and the second electromagnetic generating component are electromagnets, and the first electromagnetic absorbing component is made of stainless steel and is arranged at the front and the rear of the smoke catcher, or is a stainless steel patch attached to the front and the rear of the smoke catcher.
Preferably, the fixed structure and the moving structure each comprise a vacuum pump;
one end of the moving structure and one end of the fixed structure are both provided with adsorption holes connected with the vacuum pump;
the other end of the moving structure and the other end of the fixed structure are respectively used for adsorbing the front part of the smoke catcher and the rear part of the smoke catcher.
Preferably, the fixed structure and the moving structure further comprise a clamping jaw;
one end of the moving structure and one end of the fixed structure are both provided with adsorption holes connected with the vacuum pump;
and the other ends of the moving structure and the fixed structure are respectively provided with a clamping claw which is used for clamping the front part of the smoke catcher and the rear part of the smoke catcher.
More preferably, the motion structure further comprises a separation rod, one end of the separation rod is provided with an adsorption hole connected with the vacuum pump, and the other end of the separation rod is connected with a clamping claw.
It should be noted that the vacuum pump pumps the inside of the moving structure and the fixed structure into negative pressure through the adsorption holes, the moving structure moves downwards to the front part of the smoke catcher to separate the moving structure from the rear part, and the fixed structure further fixes the rear part of the smoke catcher due to the negative pressure formed inside, so that the rear part of the smoke catcher is ensured not to move upwards along with the front part of the smoke catcher. Furthermore. Through set up the clamping jaw at the one end of motion structure and fixed knot structure, when having increased the fixity of fume trap rear portion, can further guarantee effectual with fume trap front and back portion separation.
More preferably, the power device is, but not limited to, a paddle, a pump and a vibrator, and drives the extraction solution to flow.
Preferably, the device also comprises a liquid inlet valve and a liquid outlet valve;
the liquid inlet valve and the liquid outlet valve are both arranged on the outer bottom surface of the closed container;
the liquid inlet valve is used for injecting an extraction solution into the closed container, and the liquid outlet valve is used for taking out the extraction solution from the closed container.
Preferably, the sealing device further comprises an exhaust port, and the exhaust port is arranged on the outer top surface of the closed container.
The extraction solution can be conveniently injected into and taken out of the cigarette smoke extraction device by arranging the air outlet, and the air outlet is kept in a closed state during the operation of the cigarette smoke extraction device.
The invention also provides a cigarette smoke extraction method, which comprises the following steps:
step 1: smoking cigarettes by adopting a smoking machine, and trapping the cigarettes by adopting a smoke catcher;
step 2: placing the smoke catcher in a closed container, separating the front part of the smoke catcher from the rear part of the smoke catcher by a moving structure, injecting an extraction solution into the closed container through a liquid inlet valve, and starting a power device to enable the extraction solution to flow;
and step 3: and discharging the extraction solution through the liquid outlet valve, taking out the flue gas catcher, and carrying out gas chromatography on the extraction solution.
It should be noted that the upper part and the lower part of the flue gas catcher are separated, so that the extraction solution can be fully contacted with the glass fiber filter disc in the flue gas catcher, and in the step 2, the surface of the flue gas catcher, which is not contacted with the flue gas, is ensured to be smooth, and the whole flue gas catcher is arranged in a closed container.
More preferably, the cigarette includes a conventional cigarette, a heat non-burning cigarette and an electronic cigarette.
Further preferably, the cigarette is a cigarette which is not burned by heating.
More preferably, the smoking machines comprise linear smoking machines and carousel smoking machines.
Further preferably, the smoking machine is a linear smoking machine.
Preferably, the extraction solution is an internal standard solution;
the solvent of the internal standard solution comprises one or more of methanol, ethanol, isopropanol, dichloromethane, ethyl acetate and acetonitrile.
More preferably, the solvent of the internal standard solution is isopropanol.
Preferably, the extraction time is 1-180min.
More preferably, the time of extraction is 5min.
Preferably, the volume of the extraction solution is 2-100mL.
More preferably, the volume of the extraction solution is 70mL.
More preferably, the rotation speed of the closed vessel is 10 to 20000rpm, and still more preferably 1000rpm.
More preferably, the flue gas catcher comprises a catcher and a glass fiber filter sheet arranged in the catcher;
the diameter of the glass fiber filter disc is 1-150mm.
More preferably, the diameter of the glass fiber filter sheet is 44mm.
More preferably, each of said glass fiber filters captures between 2 and 20 cigarettes.
Further preferably, each of said glass fiber filters traps 5 cigarettes.
The invention provides a cigarette smoke extraction device and a method, which finish extraction in a closed environment, are slightly influenced by the outside, adopt a power device to provide power to enable the extraction solution and a smoke catcher to generate high-speed irregular relative motion, and have the advantages of simple operation, high extraction efficiency and good extraction effect. The cigarette smoke extraction device and the method provided by the embodiment of the invention can realize accurate determination of the moisture in the total particulate matter of the heated non-combustible cigarette, and avoid the defects of low determination result and low moisture value caused by water dispersion and residue on a smoke catcher, and high calculated NFPDM value and other (TPM-moisture-propylene glycol-glycerol-nicotine).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural view of a cigarette smoke extraction device provided in embodiment 1 of the present invention;
FIG. 2 is a schematic diagram of a method for extracting cigarette smoke from a cigarette according to embodiment 1 of the present invention;
FIG. 3 is a schematic structural view of a cigarette smoke extraction device provided in embodiment 2 of the present invention;
FIG. 4 is a schematic diagram of a method for extracting cigarette smoke from a cigarette according to embodiment 2 of the present invention;
FIG. 5 is a schematic structural view of a cigarette smoke extraction device provided in embodiment 3 of the present invention;
FIG. 6 is a schematic diagram of a method for extracting cigarette smoke from a cigarette according to embodiment 3 of the present invention;
wherein the reference numbers are as follows:
the smoke catcher comprises a smoke catcher front part 1, a smoke catcher rear part 2, a second electromagnetism generating part 3, a first electromagnetism generating part 4, a closed container 5, a separating rod 6, a stirring part 7, a liquid inlet and outlet valve 8, an exhaust port 9, an extraction liquid 10 and a cigarette holder 11.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a cigarette smoke extraction device and method, and solves the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
The cigarette smoke extraction device and method provided by the embodiment of the invention are further explained below.
Example 1
Referring to fig. 1, a first embodiment of a cigarette smoke extraction device according to the present invention includes a smoke catcher, a moving structure, a fixed structure, a sealed container 5, and a power device.
The flue gas catcher is arranged in the closed container 5;
the fixed structure is used for fixing the rear part 2 of the smoke catcher;
the motion structure is used for separating the front part 1 of the smoke catcher from the rear part 2 of the smoke catcher in the closed container 5;
the power device is used for driving the extraction solution to flow in the closed container 5.
The cigarette smoke extraction device provided by the embodiment of the invention finishes extraction in a closed environment, is slightly influenced by the outside, adopts the power device to provide power to enable the extraction solution and the smoke catcher to generate high-speed irregular relative motion, and has the advantages of simple operation, high extraction efficiency and good extraction effect.
Further, in the present embodiment, the moving structure and the fixed structure are the separation rod 6 on which the first electromagnetic generating part 4 is mounted and the second electromagnetic generating part 3, respectively.
A first electromagnetic adsorption component and a second electromagnetic adsorption component are respectively arranged at the front part 1 and the rear part 2 of the smoke catcher;
the first electromagnetic generating component 4 and the second electromagnetic generating component 3 are magnetically connected to the first electromagnetic attracting component and the second electromagnetic attracting component, respectively.
Further, the first electromagnetic generating member 4 and the second electromagnetic generating member 3 are both electromagnets.
Furthermore, in this embodiment, the power device is a closed container 5 having a stirring member 7 mounted on an inner wall thereof, and the stirring member 7 rotates and drives the extraction solution to flow.
Further, the device also comprises a liquid inlet valve and a liquid outlet valve;
the liquid inlet valve and the liquid outlet valve are both arranged on the outer bottom surface of the closed container 5;
the liquid inlet valve is used for injecting an extraction solution into the closed container 5, and the liquid outlet valve is used for taking out the extraction solution from the closed container 5.
Furthermore, in this embodiment, the liquid inlet valve and the liquid outlet valve are liquid inlet and outlet valves 8, and the liquid inlet and outlet valves 8 are used for injecting the extraction solution into the container portion and discharging the extraction solution from the container portion;
further, the air outlet 9 is also included, and the air outlet 9 is arranged on the outer top surface of the closed container 5.
Referring to fig. 2, an embodiment of the present invention further provides an extraction method based on the cigarette smoke extraction device in this embodiment, which specifically includes the following steps:
step 1: the cigarettes are smoked by adopting a linear smoking machine, wherein the smoking curve is bell-shaped, the smoking capacity is 35 +/-0.3 mL, the smoking duration is 2s, the smoking interval is 30s, glass fiber filter discs with the diameter of 44mm are adopted to collect the particulate matter components of the smoke of the cigarettes, and each filter disc collects 5 cigarettes.
And 2, step: the smoke catcher is taken down from the linear type smoking machine, the cigarette holder 11 on the smoke catcher is removed, the whole smoke catcher is arranged in the closed container 5, the rear part 2 of the smoke catcher is fixed through the fixed structure of the closed container 5, wherein the moving structure and the fixed structure are respectively the separating rod 6 with the first electromagnetic generating component 4 mounted at the top and the second electromagnetic generating component 3. The first electromagnetic generating member 4 and the second electromagnetic generating member 3 are both electromagnets.
The separation rod 6 moves downwards until contacting with the front part 1 of the smoke catcher, the upper electromagnet and the lower electromagnet are electrified, when the rear part 2 of the smoke catcher is adsorbed by the electromagnet below, the separation rod 6 moves upwards and adsorbs the front part 1 of the smoke catcher to move upwards, so that the smoke catcher is opened in the closed container 5, the exhaust port 9 and the liquid inlet and outlet valve 8 are opened, 70mL of internal standard solution is injected into the smoke catcher through the liquid inlet and outlet valve 8, wherein the internal standard substances of the internal standard solution are ethanol, quinoline and 1, 4-butanediol, the solvent is isopropanol, the liquid inlet and outlet valve 8 and the exhaust port 9 are closed, the closed container 5 is started, the stirring piece 7 on the inner wall of the closed container drives the extraction solution to generate high-speed vortex motion, extraction is performed for 5min to obtain extraction liquid 10, and the extraction liquid 10 is taken through the liquid inlet and outlet valve 8 and passes through a 0.45 mu m organic phase filter membrane after standing and is operated on a machine for analysis.
And step 3: performing gas chromatography with double columns and double detectors, wherein the system A is used for determining water content, the chromatographic column is a packed column, and the stationary phase is Porapak Q 2 (150 μm), the detector is a TCD detector; the B system was used for the determination of nicotine, 1, 2-propanediol and glycerol, the column was DB-WAXETR (30 m. Times.0.32mm, 1 μm) and the detector was FID detector.
Wherein the injection port temperature of the system A is 150 ℃, and the carrier gas is nitrogen (N) with the flow rate of 5mL/min 2 ) The sample injection volume is 0.5 mu L, the sample injection mode is non-split flow sample injection, and the temperature of the detector is 250 ℃.
Sample inlet temperature of system B: n at 250 ℃ and a carrier gas flow rate of 0.7mL/min 2 The sample introduction volume is 1 mu L, the sample introduction mode adopts split sample introduction, the split ratio is 30 2 The detector temperature was 275 deg.C, the flow rate of hydrogen was 30mL/min, and the flow rate of air was 400mL/min.
Different electric heating devices are adopted to respectively heat the adaptive non-burning cigarette rods, a glass fiber filter disc is used for trapping aerosol particulate matters, the total weight of the smoke trap before and after smoking is respectively measured, and the difference value is calculated to obtain the Total Particulate Matter (TPM). After smoking the cigarettes, extracting water, nicotine, 1, 2-propylene glycol and glycerol in the glass fiber filter disc by using an extraction solution containing an internal standard (circulation extraction), then analyzing by using a GC-TCD (gas chromatography thermal conductivity detector) and a GC-FID (gas chromatography hydrogen flame ionization detector), and quantifying by using an internal standard method, wherein the internal standard of the water is ethanol, the internal standard of the nicotine is quinoline, the internal standard of the 1, 2-propylene glycol and the glycerol is 1, 4-butanediol, and the measurement results are shown in Table 1.
TABLE 1 Total particulate matter of aerosol of non-combustible cigarette, moisture, nicotine, 1, 2-propylene glycol and glycerin measured in example 1
Note: other = TPM-moisture-nicotine-1, 2-propanediol-glycerol
Example 2
Referring to fig. 3 and 4, the difference between the cigarette smoke extracting apparatus and method provided in embodiment 2 and embodiment 1 is that the stirring member 7 in embodiment 2 is a pump, and the pump drives the closed container 5 and the extracting solution to make a vibrating motion.
The analysis and detection are carried out on the cigarettes which are not combusted in different heating modes in the embodiment 2, and the results are shown in the table 2:
TABLE 2 measurement results of aerosol total particulate matter, moisture, nicotine, 1, 2-propylene glycol and glycerin of the cigarette subjected to different heating and non-combustion in example 2
Example 3
Referring to fig. 5 and 6, the difference between the cigarette smoke extracting apparatus and method provided in embodiments 3 and 1 is that the stirring member 7 in embodiment 3 is a vibrating device, and the vibrating device is fixedly connected to the outside of the sealed container 5 and drives the sealed container 5 and the extracting solution to vibrate.
The analysis and detection are carried out on the cigarettes which are not combusted in different heating modes in the embodiment 3, and the results are shown in the table 3:
TABLE 3 Total particulate matter of aerosol of non-combustible cigarette by different heating and measurement results of moisture, nicotine, 1, 2-propanediol and glycerol in example 3
Comparing the analytical test results of the above examples with the conventional cigarette extraction method, table 4 is obtained:
TABLE 4 results of determination of water, nicotine, propylene glycol and glycerol in total particulate matter of non-burning cigarette by different extraction methods
As can be seen from comparison of data in tables 1 to 4, in the method for extracting cigarette smoke provided in the embodiment of the present invention, the smoke trap is integrally placed in the closed container 5, and the stirring member 7 drives the extraction solution to vibrate, so that the problem of inaccurate measurement result caused by volatilization of smoke components, component residue of the smoke trap, and the like in the process of taking out a glass fiber filter in the prior art is avoided, accurate measurement of water in the total particulate matter of a cigarette which is not heated and combusted is realized, and the defects of low measurement result and low water value caused by water dispersion and residue on the smoke trap in the conventional method that the NFPDM value obtained by calculation is higher than that of other (TPM-water-propylene glycol-glycerol-nicotine) are avoided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that various modifications of the embodiments can be implemented by those skilled in the art without departing from the technical principle of the present invention, and these modifications should be regarded as the scope of the present invention.
Claims (6)
1. A cigarette smoke extraction device is characterized by comprising a smoke catcher, a separation structure, a closed container, a power device and a liquid outlet valve;
the smoke catcher is arranged in the closed container and comprises a smoke catcher front part and a smoke catcher rear part;
the separation structure is used for separating the front part of the smoke catcher from the rear part of the smoke catcher;
the power device is used for driving the extraction solution to flow in the closed container;
the liquid outlet valve is arranged on the outer bottom surface of the closed container and is used for taking the extraction solution out of the closed container;
the separation structure comprises a fixed structure and a moving structure, the fixed structure is used for fixing the rear part of the smoke catcher, and the moving structure is used for separating the front part of the smoke catcher from the rear part of the smoke catcher;
the moving structure comprises a separating rod and a first motor, the top of the separating rod is provided with a first electromagnetic generating component, and the fixed structure comprises a second electromagnetic generating component;
the front part of the smoke catcher and the rear part of the smoke catcher are respectively provided with a first electromagnetic adsorption part and a second electromagnetic adsorption part;
the first motor drives the first electromagnetic generating component to move to the first electromagnetic adsorption component, so that the first electromagnetic generating component is magnetically connected with the first electromagnetic adsorption component;
the second electromagnetic generating component is magnetically connected with the second electromagnetic adsorbing component;
or, the fixed structure and the moving structure both comprise a vacuum pump and a clamping jaw;
one end of the moving structure and one end of the fixed structure are both provided with adsorption holes connected with the vacuum pump;
the other end of the moving structure and the other end of the fixed structure are respectively used for adsorbing the front part of the smoke catcher and the rear part of the smoke catcher;
the other end of the moving structure and the other end of the fixed structure are both provided with the clamping claws, and the clamping claws are used for clamping the front part of the smoke catcher and the rear part of the smoke catcher.
2. The cigarette smoke extraction device of claim 1, further comprising a liquid inlet valve; the liquid inlet valve is arranged on the outer bottom surface of the closed container and used for injecting extraction solution into the closed container.
3. The cigarette smoke extraction device of claim 1, further comprising an air vent disposed on an outer top surface of the closed container.
4. A cigarette smoke extraction method, which is applied to the cigarette smoke extraction device according to any one of claims 1 to 3, and comprises the following steps:
step 1: smoking cigarettes by using a smoking machine, and trapping the cigarettes by using a smoke catcher;
step 2: placing the smoke catcher in a closed container, separating the front part of the smoke catcher from the rear part of the smoke catcher by a motion structure, injecting an extraction solution into the closed container through a liquid inlet valve, and starting a power device to enable the extraction solution to generate irregular motion;
and step 3: and discharging the extraction solution through a liquid outlet valve, taking out the flue gas catcher, and carrying out gas chromatography on the extraction solution.
5. The cigarette smoke extraction method of claim 4, wherein the extraction solution is an internal standard solution;
the solvent of the internal standard solution comprises one or more of methanol, ethanol, isopropanol, dichloromethane, ethyl acetate and acetonitrile.
6. The cigarette smoke extraction method of claim 4, wherein the time of the irregular movement is 1-180 min;
the volume of the extraction solution is 2-100mL.
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