CN113970601A - On-line analysis and detection device and method for smoke of heated cigarette - Google Patents
On-line analysis and detection device and method for smoke of heated cigarette Download PDFInfo
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- CN113970601A CN113970601A CN202010717212.7A CN202010717212A CN113970601A CN 113970601 A CN113970601 A CN 113970601A CN 202010717212 A CN202010717212 A CN 202010717212A CN 113970601 A CN113970601 A CN 113970601A
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Images
Classifications
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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
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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
Abstract
The invention discloses a heated cigarette smoke on-line analysis and detection device and a method, wherein the device comprises a cigarette holder, a cigarette suction module, a sample quantification ring, an internal standard sample quantification ring, a ten-way valve, an on-line smoke analysis module, a flow path system and a control module; the cigarette holder, the cigarette suction module, the sample quantitative ring, the internal standard sample quantitative ring and the on-line smoke analysis module are all communicated with the ten-way valve through a flow path system; the cigarette holder, the cigarette suction module, the ten-way valve, the online smoke analysis module and the flow path system are all controlled by the control module; the sample quantitative ring is used for collecting a flue gas sample; the internal standard sample quantitative ring is used for collecting an internal standard gas sample; the online flue gas analysis module is used for receiving the flue gas sample and the internal standard gas sample to perform on-line flue gas analysis and detection. The internal standard gas is quantitatively introduced into the online flue gas analysis module through the online introduction of the internal standard module, so that the accuracy of sample introduction can be ensured, and the detection precision is improved; the flue gas sample does not need any sample pretreatment, and is simple, convenient and efficient.
Description
Technical Field
The invention relates to the technical field of on-line analysis of smoke of heated cigarettes, in particular to a device and a method for on-line analysis and detection of smoke of heated cigarettes.
Background
In recent years, Heated Tobaccos (HTPs) are heated (200-350 ℃) by an external heat source without directly burning cigarettes, so that harmful components generated by combustion and cracking of tobaccos at high temperature (up to 900 ℃) are reduced, the taste of the heated cigarettes is most similar to that of traditional cigarettes, and the heated cigarettes are favored by consumers.
The smoke is the most important characteristic of the tobacco products facing consumers, is the most important factor for reflecting the quality level and the style characteristics of the tobacco products, and the analysis of the chemical components of the smoke is very important basic research work. Heated cigarettes produce aerosols by means of heated distillation, the smoke of which may contain less material derived from the pyrolysis and combustion of tobacco, but which may promote the release of those thermally distillable compounds into the aerosol stream. In view of the above, there is a need to analyze the smoke of heated cigarettes to reveal the release profile and mechanism of the smoke. At present, the method for analyzing the smoke of the heated cigarette mainly adopts a Cambridge filter disc to capture the smoke, and then adopts pretreatment processes such as solvent extraction or solid phase extraction to process a sample, the off-line analysis method has the disadvantages of complex operation, time consumption and labor consumption, and the long-time pretreatment process can also cause volatile substances, particularly high volatile substances to volatilize and escape. In order to solve the problems, some online analysis technologies, mainly an online mass spectrometry technology with a soft ionization technology as a core, have been tried in the research of cigarette smoke analysis. However, the research on the on-line analysis method of the smoke of the heated cigarette is still blank.
Disclosure of Invention
The invention provides a device and a method for on-line analysis and detection of smoke of a heated cigarette, which are used for realizing real-time on-line detection of the smoke of the heated cigarette.
In order to achieve the above object, the present invention provides the following technical solutions.
In a first aspect, the on-line analysis and detection device for the smoke of the heated cigarette comprises a cigarette holder, a cigarette smoking module, a sample quantification ring, an internal standard sample quantification ring, a ten-way valve, an on-line smoke analysis module, a flow path system and a control module;
the cigarette holder, the cigarette suction module, the sample quantitative ring, the internal standard sample quantitative ring and the on-line smoke analysis module are all communicated with the ten-way valve through a flow path system, and the ten-way valve is also used for being communicated with external carrier gas;
the cigarette holder, the cigarette suction module, the ten-way valve, the online smoke analysis module and the flow path system are all controlled by the control module; wherein the content of the first and second substances,
the sample quantitative ring is used for collecting a flue gas sample and loading the flue gas sample into the online flue gas analysis module through carrier gas;
the internal standard sample quantitative ring is used for collecting an internal standard gas sample and loading the internal standard gas sample into the online smoke analysis module through carrier gas;
the online smoke analysis module is used for receiving the smoke sample and the internal standard gas sample to perform smoke online analysis and detection.
The existing smoke analysis basically adopts an off-line method, an internal standard solution is added, even if the off-line analysis is improved, the internal standard solution is also added like the off-line method, firstly, the internal standard solution is added into a cigarette sample, but the problem that the release amount of the internal standard sample along with the cigarette suction is involved (the content is uncertain), and the detection result is inaccurate; in the invention, the internal standard sample quantifying ring is introduced, the internal standard substance is directly made into the standard gas, and the internal standard gas is quantitatively introduced into the on-line flue gas analysis module through the internal standard sample quantifying ring, so that the accuracy of sample introduction can be ensured, the analysis error is reduced, and the measurement precision of an instrument is improved; on the other hand, the analysis accuracy can be improved, including difference comparison and semi-quantitative analysis. The flue gas sample collected in the sample quantitative ring is directly and rapidly transferred to the on-line flue gas analysis module for analysis in a nondestructive mode without any sample pretreatment, so that the complex treatment process in an off-line analysis method is avoided, the chemical substance information of the whole flue gas (particle phase matter and gas phase matter) can be obtained in one step, and the method has the advantages of simplicity, convenience and high efficiency. In addition, because the tar content in the smoke of the heated cigarette is much lower than that of the traditional cigarette, and the pollution to the pipeline is less in the smoke analysis process, the invention can remove the residue adsorbed by the pipeline only by adopting a gas purging mode, thereby avoiding the use of toxic organic solvents. By controlling the ten-way valve, sampling and sample introduction of the smoke gas and the internal standard gas can be realized, the structure is simple, the cost is low, and the failure rate can be reduced.
Furthermore, the flow path system comprises a flow regulating valve and a plurality of pipelines;
when the ten-way valve is in a first state, the cigarette holder, the sample quantifying ring and the cigarette suction module are sequentially connected through the ten-way valve and a plurality of pipelines, the external internal standard gas, the internal standard sample quantifying ring and the sampling pump are sequentially connected through the ten-way valve and the plurality of pipelines, and the external carrier gas, the flow regulating valve and the online smoke analysis module are sequentially connected through the ten-way valve and the plurality of pipelines;
when the ten-way valve is in the second state, the cigarette holder and the cigarette suction module are sequentially connected through the ten-way valve and the plurality of pipelines, the external carrier gas, the flow regulating valve, the internal standard sample quantifying ring, the sample quantifying ring and the online smoke analysis module are sequentially connected through the ten-way valve and the plurality of pipelines, and the external internal standard gas and the sampling pump are sequentially connected through the ten-way valve and the plurality of pipelines.
Can constitute online sampling module through sample ration ring with ten logical valve, can constitute and introduce interior mark module on line through interior mark sample ration ring with ten logical valve, only can realize the sampling and the appearance of advance of flue gas and interior mark gas through control module control ten logical valve switching state, and can guarantee to advance the accuracy of appearance volume, reduce the analysis error, improve instrument measurement precision, and simple structure.
Further, the flue gas absorption device also comprises a residual flue gas absorption module, and the flow path system also comprises a first two-position three-way electromagnetic valve;
a first port of the first two-position three-way electromagnetic valve is communicated with the residual smoke absorption module, a second port of the first two-position three-way electromagnetic valve is communicated with the ten-way valve, and a third port of the first two-position three-way electromagnetic valve is communicated with the cigarette suction module;
when the first two-position three-way electromagnetic valve is in a first state, the second port is communicated with the third port, and when the first two-position three-way electromagnetic valve is in a second state, the first port is communicated with the third port.
In the sampling process of the smoke and the internal standard gas, the first two-position three-way electromagnetic valve is in a first state and is communicated with a smoke suction pipeline; in the sample introduction process, the control module controls the first two-position three-way electromagnetic valve to be switched into the second state, and the cigarette suction module is conducted with the first port at the moment, so that smoke in the cigarette suction module can be discharged in time. If the smoke is directly discharged into indoor ambient air, environmental pollution is easily caused; meanwhile, the cigarette can also suck indoor air when being sucked, and the detection result is possibly influenced; the exhaust smoke is filtered by additionally arranging the residual smoke absorption module, so that the detection result can be further ensured, and the smoke absorption device is more environment-friendly.
Further, the residual flue gas absorption module comprises an adsorption tube and an adsorbent filled in the adsorption tube, one end of the adsorption tube is communicated with the first port, and the other end of the adsorption tube is evacuated. The structure of the adsorption tube and the filled adsorbent can be conveniently replaced after the adsorbent is adsorbed and saturated.
Furthermore, the adsorbent is one or more of activated carbon, graphitized carbon black and molecular sieve, and polyethylene sieve plates are filled at two ends of the adsorbent.
Further, the sample quantification loop volume is 0.5-3mL, and the internal standard sample quantification loop volume is 0.25-1 mL.
Further, the internal standard substance of the internal standard gas is one or more of ethanol, deuterated benzene, deuterated toluene, deuterated o-xylene and deuterated p-xylene, and the concentration of the internal standard gas is 1-500 ppm.
Considering that the internal standard gas is required to be used for detection, the internal standard substance of the internal standard gas needs to be some substances which are easy to gasify to prepare standard gas, and the stability of the internal standard gas is good.
Further, the on-line flue gas analysis module comprises one of a gas chromatograph, a gas chromatograph-mass spectrometer, an on-line mass spectrum and an ion mobility spectrometer, and is also communicated with external carrier gas.
Furthermore, the cigarette suction module comprises a suction needle cylinder and a motor for driving a piston in the suction needle cylinder to reciprocate; the cigarette suction module has the parameters as follows: the suction curve is one of bell shape, triangle shape and rectangle shape, the suction capacity is 5-150mL, the suction duration is 0.8-10s, and the suction interval is 15-120 s.
Furthermore, the ten-way valve, the sample quantitative ring, the connecting pipeline between the cigarette holder and the ten-way valve, the connecting pipeline between the cigarette smoking module and the ten-way valve, and the connecting pipeline between the ten-way valve and the on-line smoke analysis module are all arranged in the heating and heat preservation box, and the heating and heat preservation temperature is 40-300 ℃. Because some substances in the flue gas have higher boiling points and are easy to be adsorbed on the pipe wall, all the pipelines adopt inert stainless steel pipes, and the heating and heat preservation are carried out on all the pipelines, the ten-way valve and the sample quantitative ring, so that the condensation adsorption of the flue gas can be reduced, and the flue gas has little or no residue after passing through the pipelines. The pollution problem caused by pipeline residue and the like is avoided, and the problem of low analysis precision caused by cross contamination is reduced.
In a second aspect, an online analysis and detection method for heated cigarette smoke is provided, which is characterized in that the online analysis and detection device for heated cigarette smoke is adopted for online analysis and detection, and comprises the following steps:
inserting the heated cigarette into a cigarette holder and heating;
starting a cigarette suction module, and collecting a smoke sample with a preset volume by a sample quantifying ring in the smoke suction process;
pumping the internal standard gas into an internal standard sample quantifying ring, and collecting an internal standard gas sample with a preset volume by the internal standard sample quantifying ring;
and loading the flue gas sample and the internal standard gas sample into an online flue gas analysis module through carrier gas to perform online flue gas analysis and detection.
Further, still include:
when the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module through carrier gas, the smoke in the cigarette suction module is discharged;
after the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module, the online smoke analysis module is disconnected from the flow path system, carrier gas is introduced to purge the sample quantification ring, the internal standard sample quantification ring, the ten-way valve and a pipeline between the ten-way valve and the online smoke analysis module, and the cigarette suction module is started to extract ambient air to purge the pipelines between the cigarette holder and the ten-way valve and between the ten-way valve and the cigarette suction module.
Advantageous effects
The invention provides an on-line analysis and detection device and method for smoke of a heated cigarette, wherein a smoke sample collected in an on-line sampling module is directly and rapidly transferred to an on-line smoke analysis module for analysis without any sample pretreatment in a nondestructive mode, so that a complex treatment process in an off-line analysis method is avoided, chemical substance information of whole smoke (particle phase substances and gas phase substances) can be obtained in one step, and the device and method have the advantages of simplicity, convenience and high efficiency. Particularly, the existing smoke analysis basically adopts an off-line method, and an internal standard solution is added, so that even if the existing smoke analysis is improved to on-line analysis, the internal standard solution is added like the off-line method, firstly, the internal standard solution is added into a cigarette sample, but the problem that the release amount of the internal standard sample along with the cigarette smoking is involved (the content is uncertain), and the detection result is inaccurate; in the invention, the internal standard sample quantifying ring is introduced, the internal standard substance is directly made into the standard gas, and the internal standard gas is quantitatively introduced into the on-line flue gas analysis module through the internal standard sample quantifying ring, so that the accuracy of sample introduction can be ensured, the analysis error is reduced, and the measurement precision of an instrument is improved; on the other hand, the analysis accuracy can be improved, including difference comparison and semi-quantitative analysis. In addition, because the tar content in the smoke of the heated cigarette is much lower than that of the traditional cigarette, and the pollution to the pipeline is less in the smoke analysis process, the invention can remove the residue adsorbed by the pipeline only by adopting a gas purging mode, thereby avoiding the use of toxic organic solvents. By controlling the ten-way valve, sampling and sample introduction of the smoke gas and the internal standard gas can be realized, the structure is simple, the cost is low, and the failure rate can be reduced.
Drawings
FIG. 1 is a schematic structural diagram of an on-line analysis and detection device for smoke of a heated cigarette provided by an embodiment of the present invention;
FIG. 2 is a schematic diagram of the gas path of the embodiment provided in FIG. 1 in a cigarette smoking-smoke collection-internal standard gas collection state;
FIG. 3 is a schematic diagram of the gas path of the embodiment provided in FIG. 1 in a state of flue gas injection-internal standard gas injection;
FIG. 4 is a schematic view of the gas path of the embodiment provided in FIG. 1 in a line purge condition;
fig. 5 is a total ion flow diagram for detecting total smoke (port 3) of a commercially available heated cigarette according to an embodiment of the present invention.
In the figure: 100-a cigarette holder, 200-a cigarette suction module, 201-a suction needle cylinder, 202-a piston, 203-a motor, 302-a sample quantification ring, 401-an internal standard sample quantification ring, 500-an online smoke analysis module, 600-a residual smoke absorption module, 601-an adsorbent, 602-an adsorption tube, 701-a gas carrying pipeline, 702-a sample introduction pipeline, 703-a first two-position three-way electromagnetic valve, 704-a second two-position three-way electromagnetic valve, 705-a flow regulating valve and 800-a ten-way valve.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, the present embodiment provides an online analysis and detection device for smoke of a heated cigarette, which includes a cigarette holder 100, a cigarette smoking module 200, a sample quantifying ring 302, an internal standard sample quantifying ring 401, a ten-way valve 800, an online smoke analysis module 500, a flow path system, and a control module;
the cigarette holder 100, the cigarette suction module 200, the sample quantitative ring 302, the internal standard sample quantitative ring 401 and the online smoke analysis module 500 are all communicated with the ten-way valve 800 through a flow path system, and the ten-way valve 800 is also used for being communicated with external carrier gas;
the cigarette holder 100, the cigarette suction module 200, the ten-way valve 800, the online smoke analysis module 500 and the flow path system are all controlled by the control module; wherein the content of the first and second substances,
the sample quantitative ring 302 is used for collecting a flue gas sample and loading the flue gas sample into the online flue gas analysis module 500 through a carrier gas;
the internal standard sample quantifying ring 401 is used for collecting an internal standard gas sample and loading the internal standard gas sample into the online flue gas analysis module 500 through carrier gas;
the online flue gas analysis module 500 is used for receiving a flue gas sample and an internal standard gas sample to perform online flue gas analysis and detection.
The existing smoke analysis basically adopts an off-line method, an internal standard solution is added, even if the off-line analysis is improved, the internal standard solution is also added like the off-line method, firstly, the internal standard solution is added into a cigarette sample, but the problem that the release amount of the internal standard sample along with the cigarette suction is involved (the content is uncertain), and the detection result is inaccurate; in the invention, the internal standard sample quantifying ring is introduced, the internal standard substance is directly made into the standard gas, and the internal standard gas is quantitatively introduced into the on-line flue gas analysis module through the internal standard sample quantifying ring, so that the accuracy of sample introduction can be ensured, the analysis error is reduced, and the measurement precision of an instrument is improved; on the other hand, the analysis accuracy can be improved, including difference comparison and semi-quantitative analysis. The flue gas sample collected in the sample quantitative ring is directly and rapidly transferred to the on-line flue gas analysis module for analysis in a nondestructive mode without any sample pretreatment, so that the complex treatment process in an off-line analysis method is avoided, the chemical substance information of the whole flue gas (particle phase matter and gas phase matter) can be obtained in one step, and the method has the advantages of simplicity, convenience and high efficiency. In addition, because the tar content in the smoke of the heated cigarette is much lower than that of the traditional cigarette, and the pollution to the pipeline is less in the smoke analysis process, the invention can remove the residue adsorbed by the pipeline only by adopting a gas purging mode, thereby avoiding the use of toxic organic solvents. By controlling the ten-way valve, sampling and sample introduction of the smoke gas and the internal standard gas can be realized, the structure is simple, the cost is low, and the failure rate can be reduced.
Specifically, the flow path system includes a flow regulating valve 705 and a plurality of pipelines;
when the ten-way valve 800 is in the first state, the cigarette holder 100, the sample quantifying ring 302 and the cigarette smoking module 200 are sequentially connected through the ten-way valve 800 and a plurality of pipelines, the external internal standard gas, the internal standard sample quantifying ring 401 and the sampling pump are sequentially connected through the ten-way valve 800 and a plurality of pipelines, and the external carrier gas, the flow regulating valve 705 and the online smoke analysis module 500 are sequentially connected through the ten-way valve 800 and a plurality of pipelines;
when the ten-way valve 800 is in the second state, the cigarette holder 100 and the cigarette suction module 200 are sequentially connected through the ten-way valve 800 and a plurality of pipelines, the external carrier gas, the flow regulating valve 705, the internal standard sample quantifying ring 401, the sample quantifying ring 302 and the online smoke analysis module 500 are sequentially connected through the ten-way valve 800 and the plurality of pipelines, and the external internal standard gas and the sampling pump are sequentially connected through the ten-way valve 800 and the plurality of pipelines.
More specifically, as shown in fig. 1, the cigarette holder 100 is connected to the port 8-1 of the ten-way valve 800, the cigarette smoking module 200 is connected to the port 8-2 of the ten-way valve 800, the two ends of the sample quantifying ring 302 are respectively connected to the ports 8-3 and 8-10 of the ten-way valve 800, the online smoke analyzing module 500 is connected to the ports 8-9 of the ten-way valve 800, the two ends of the internal standard sample quantifying ring 401 are respectively connected to the ports 8-4 and 8-7 of the ten-way valve 800, the ports 8-6 and 8-5 of the ten-way valve 800 are respectively connected to the sampling pump and the external internal standard gas, and the 5-2 end of the flow regulating valve 705 is connected to the ports 8-8 of the ten-way valve 800. A pipeline between the flow regulating valve 705 and external carrier gas is a carrier gas pipeline 701, and the 5-1 end of the flow regulating valve 705 is communicated with the carrier gas pipeline 701 to form a carrier gas inlet; the pipeline between the on-line flue gas analysis module 500 and the ports 8-9 of the ten-way valve 800 is a sample inlet pipeline 702, and the sample inlet pipeline 702 is communicated with the ports 8-9 of the ten-way valve 800 to form a sample gas inlet.
When the ten-way valve 800 is in the first state, the port communication state of the ten-way valve 800 is: port 8-1 communicates with port 8-10, port 8-2 communicates with port 8-3, port 8-4 communicates with port 8-5, port 8-6 communicates with port 8-7, and port 8-8 communicates with port 8-9. When the ten-way valve 800 is in the second state, the port communication state of the ten-way valve 800 is: port 8-1 communicates with port 8-2, port 8-3 communicates with port 8-4, port 8-5 communicates with port 8-6, port 8-7 communicates with port 8-8, and port 8-9 communicates with port 8-10.
Can constitute online sampling module through sample ration ring with ten logical valve, can constitute and introduce interior mark module on line through interior mark sample ration ring with ten logical valve, only can realize the sampling and the appearance of advance of flue gas and interior mark gas through control module control ten logical valve switching state, and can guarantee to advance the accuracy of appearance volume, reduce the analysis error, improve instrument measurement precision, and simple structure.
Preferably, the system further comprises a residual flue gas absorption module 600, and the flow path system further comprises a first two-position three-way electromagnetic valve 703;
a first port 3-1 of the first two-position three-way electromagnetic valve 703 is communicated with the residual smoke absorption module 600, a second port 3-2 of the first two-position three-way electromagnetic valve 703 is communicated with the ten-way valve 800, and a third port 3-3 of the first two-position three-way electromagnetic valve 703 is communicated with the cigarette suction module 200;
when the first two-position three-way solenoid valve 703 is in the first state, the second port 3-2 is communicated with the third port 3-3, and when the first two-position three-way solenoid valve 703 is in the second state, the first port 3-1 is communicated with the third port 3-3.
In the sampling process of the smoke and the internal standard gas, the first two-position three-way electromagnetic valve is in a first state and is communicated with a smoke suction pipeline; in the sample introduction process, the control module controls the first two-position three-way electromagnetic valve to be switched into the second state, and the cigarette suction module is conducted with the first port at the moment, so that smoke in the cigarette suction module can be discharged in time. If the smoke is directly discharged into indoor ambient air, environmental pollution is easily caused; meanwhile, the cigarette can also suck indoor air when being sucked, and the detection result is possibly influenced; the exhaust smoke is filtered by additionally arranging the residual smoke absorption module, so that the detection result can be further ensured, and the smoke absorption device is more environment-friendly.
Specifically, the residual flue gas absorption module 600 includes an absorption tube 602 and an adsorbent 601 filled therein, one end of the absorption tube 602 is communicated with the first port 3-1, and the other end of the absorption tube 602 is evacuated. The structure of the adsorption tube and the filled adsorbent can be conveniently replaced after the adsorbent is adsorbed and saturated. More specifically, the adsorbent 601 is one or more of activated carbon, graphitized carbon black and molecular sieve, and polyethylene sieve plates are filled at two ends of the adsorbent 601.
Preferably, the ten-way valve 800, the sample quantifying ring 302, the connecting pipeline between the cigarette holder 100 and the ten-way valve 800, the connecting pipeline between the cigarette smoking module 200 and the ten-way valve 800, and the connecting pipeline between the ten-way valve 800 and the online smoke analyzing module 500 are all arranged in the heating and heat preserving box, and the heating and heat preserving temperature is 40-300 ℃. Because some substances in the flue gas have higher boiling points and are easy to be adsorbed on the pipe wall, all the pipelines adopt inert stainless steel pipes, and the ten-way valve 800 and the sample quantifying ring 302 are heated and insulated, so that the condensation adsorption of the flue gas can be reduced, and the flue gas has little or no residue after passing through the pipelines. The pollution problem caused by pipeline residue and the like is avoided, and the problem of low analysis precision caused by cross contamination is reduced.
In specific implementation, the online flue gas analysis module 500 includes one of a gas chromatograph, a gas chromatograph-mass spectrometer, an online mass spectrometer, and an ion mobility spectrometer, and the online flue gas analysis module 500 is further communicated with an external carrier gas, and after the flue gas, an internal standard gas and other samples are loaded into the online flue gas analysis module 500, the connection between the sample injection pipeline 702 and the online flue gas analysis module 500 is disconnected, and at this time, the carrier gas is introduced into the online flue gas analysis module 500 to further load the samples into the above-mentioned instruments for detection. The cigarette suction module 200 comprises a suction needle cylinder 201 and a motor 203 for driving a piston 202 in the suction needle cylinder to reciprocate; the cigarette suction module 200 has the parameters set as follows: the suction curve is one of bell shape, triangle shape and rectangle shape, the suction capacity is 5-150mL, the suction duration is 0.8-10s, and the suction interval is 15-120 s. The volume of the sample quantification ring 302 is 0.5-3mL, and the volume of the internal standard sample quantification ring 401 is 0.25-1 mL. Considering that an internal standard gas is required for detection, the internal standard substance of the internal standard gas needs to be a substance which is easy to gasify to prepare a standard gas, and the stability of the internal standard gas is good, in this embodiment, the internal standard substance of the internal standard gas is one or more of ethanol, deuterated benzene, deuterated toluene, deuterated o-xylene and deuterated p-xylene, and the concentration of the internal standard gas is 1-500 ppm.
Optionally, in this embodiment, the flow path system further includes a second two-position three-way solenoid valve 704, a port 4-1 of the second two-position three-way solenoid valve 704 is communicated with the smoke holder 100, a port 4-3 of the second two-position three-way solenoid valve 704 is communicated with a port 1-1 of the sampling six-way valve 301, and a port 4-2 of the second two-position three-way solenoid valve 704 may be used to connect a standard gas for absolute quantification. In an initial state, a port 4-1 of the second two-position three-way solenoid valve 704 is communicated with a port 4-3; in the second state, port 4-2 of the second two-position, three-way solenoid valve 704 is in communication with port 4-3.
The embodiment also provides a heated cigarette smoke on-line analysis and detection method based on the heated cigarette smoke on-line analysis and detection device, which comprises the following steps:
inserting the heated cigarette into the cigarette holder 100 and heating;
starting the cigarette suction module 200, and collecting a smoke sample with a preset volume by the sample quantifying ring 302 in the smoke suction process;
pumping the internal standard gas into an internal standard sample quantifying ring 401, and collecting an internal standard gas sample with a preset volume by the internal standard sample quantifying ring 401;
the flue gas sample and the internal standard gas sample are loaded into the on-line flue gas analysis module 500 through the carrier gas for on-line flue gas analysis and detection.
The method further comprises the following steps:
when the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module 500 through the carrier gas, the cigarette suction module 200 discharges the smoke inside;
after the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module 500, the online smoke analysis module 500 is disconnected from the flow path system, carrier gas is introduced to purge the pipelines between the sample quantification ring 302, the internal standard sample quantification ring 401, the ten-way valve 800 and the online smoke analysis module 500, and the cigarette suction module 200 is started to extract ambient air to purge the pipelines between the cigarette holder 100 and the ten-way valve 800 and between the ten-way valve 800 and the cigarette suction module 200.
More specifically, the above method mainly includes three processes:
the method comprises the following steps of firstly, smoking cigarettes, collecting smoke and internally marking gas: the heated cigarette is inserted into the cigarette holder 100, after the appliance is triggered and preheated, the control module controls to start the cigarette smoking module 200, smoke is directly collected to the sample quantifying ring 302 in the smoking process, and meanwhile, internal standard gas is pumped into the internal standard sample quantifying ring 401. The air paths are communicated with each other as shown in FIG. 2, and the air flow direction is shown by the arrows.
The second process comprises flue gas sample injection-internal standard gas sample injection: the control module controls and switches the state of the ten-way valve 800, carrier gas enters from a gas carrying pipeline 701 and carries internal standard gas and smoke gas into the online smoke gas analysis module 500 through a sample introduction pipeline 702 for analysis, and meanwhile the control module controls and switches the state of the first two-position three-way electromagnetic valve 703, so that the smoke gas in the cigarette suction module 200 suction needle cylinder 201 is discharged and absorbed by the residual smoke gas absorption module 600. The air paths are communicated with each other as shown in FIG. 3, and the air flow direction is shown by the arrows.
And a third process of cleaning the pipeline: after the sampling of the flue gas is finished, the sampling pipeline 702 is pulled out from the on-line flue gas analysis module 500, the carrier gas enters the internal standard sample quantitative ring 401, the sample quantitative ring 302 and the pipeline from the gas carrying pipeline 701 to be blown and swept so as to remove residual flue gas, meanwhile, the control module controls and switches the state of the first two-position three-way electromagnetic valve 703, and controls and starts the cigarette suction module 200 to extract ambient air to blow and sweep the suction pipeline. The air paths are communicated with each other as shown in FIG. 4, and the air flow direction is shown by the arrows.
The heating cigarette heats the cut tobacco by an external heat source without directly burning the cigarette, the heating temperature is 200-350 ℃, and the temperature of the traditional cigarette during burning is as high as 900 ℃, so that the smoke generated by two cigarette samples has certain difference in chemical composition, and the physical properties such as aerosol particle size, particle quantity and the like are different.
Because the tar content in the traditional cigarette smoke is larger and the pollution to the pipeline is serious, the original cigarette mainstream smoke analysis system adopts a liquid washing and gas washing section to wash the pipeline, the complexity of the system is increased, the pipeline is longer, and the dead volume outside the column is larger; in addition, the cleaning solvent adopted by the platform is chloroform, so that the toxicity is high; from the environmental protection angle, the exhaust flue gas should adopt absorbing device collection processing in the experimentation, avoids environmental pollution.
Aiming at the problems, the invention adopts the research scheme that a gas sample injection valve is adopted to collect the smoke of the heated cigarette and directly inject the smoke through valve switching. Aiming at the overlong pipeline of the cigarette mainstream smoke analysis platform, the smoke sampling device is simplified; because the tar content in the smoke of the heated cigarette is much lower than that of the traditional cigarette, the pollution to the pipeline is less in the smoke analysis process, and the adsorption residue of the pipeline is removed only by adopting a gas purging mode, so that the use of toxic organic solvents is avoided; because some substances in the flue gas have high boiling points and are easy to be adsorbed on the pipe wall, all experimental pipelines adopt inert stainless steel pipes, and all pipelines and valve components are heated and insulated, so that the adsorption and residue of high-boiling-point substances are reduced; in order to improve the measuring accuracy and precision of the instrument and eliminate the influence of matrix effect, an internal standard device is additionally introduced on line; the flue gas absorption device is adopted to collect and treat the evacuated flue gas in the experimental process, so that the environmental pollution is avoided. The platform is connected with an analysis instrument through a heating transmission line and is used for measuring components in the smoke of the heated cigarette and realizing real-time and online detection of the smoke of the single-mouth heated cigarette.
The on-line introduction of the gas internal standard also involves the processes of air pressure fluctuation, gas sample uniform mixing and the like, and if the gas internal standard is directly introduced (similar to carrier gas), the pressure fluctuation is easily caused, and the operation of the instrument is influenced; the internal standard gas is quantitatively introduced by the quantitative ring, so that the problems can be avoided, the accuracy of sample injection quantity can be ensured, the analysis error is reduced, and the measurement precision of an instrument is improved; on the other hand, the analysis accuracy including contrast comparison, semi-quantitative analysis, etc. can be improved. The selection of the internal standard is different from the off-line method, the internal standard substance needs to be a substance which is easy to gasify to prepare standard gas, and the stability of the internal standard gas is required.
In order to further understand the technical solution of the present invention, the following description is further made with reference to some specific embodiments.
Example 1
And (4) detecting the whole smoke components of the heated cigarette on line.
A gas chromatograph mass spectrometer (GC/MS) is used as an analysis detector, and an online analysis device adopts the online analysis detection device shown in FIG. 1. The volume of the sample quantitative ring is 0.5mL, the internal standard gas is ethanol standard gas, the volume of the internal standard sample quantitative ring is 0.25mL, and the heat preservation temperature of the transmission pipeline is 150 ℃.
Heated cigarette sample preparation and smoking: before the experiment, the heated cigarette sample is placed under the conditions of constant temperature and constant humidity with the temperature (22 +/-1) DEG C and the relative humidity (60 +/-2)% for balancing for 48 hours. The aspiration parameters were aspiration volume 55mL, aspiration duration 2s, aspiration interval 30s, and aspiration curve bell-shaped.
GC conditions were as follows: the chromatographic column is an Agilent DB-WAXETR quartz capillary column (60m is multiplied by 250 μm is multiplied by 0.25 μm); the temperature of a sample inlet is 250 ℃; carrier gas He (purity 99.999%), flow rate 1 mL/min; the split ratio is 5: 1; the temperature rising procedure is as follows:
MS conditions: electron impact ion source (EI) temperature 230 ℃; ionization energy 70 eV; the transmission line temperature is 250 ℃; the scan range was 33-400 amu.
The specific operation steps are as follows: inserting the heated cigarette into a cigarette holder, starting a cigarette suction module after the appliance is triggered and preheated, directly collecting smoke (No. 3) to a sample quantitative ring in the suction process, and pumping internal standard gas into the internal standard sample quantitative ring; switching the state of the ten-way valve, allowing carrier gas to enter from a gas carrying pipeline, loading the internal standard gas and the smoke into a gas chromatography mass spectrometer through a sample introduction pipeline for analysis, and simultaneously switching the state of the first two-position three-way electromagnetic valve to discharge the smoke sucked into the needle cylinder by the cigarette suction module and absorb the smoke through the residual smoke absorption module; after the sampling of flue gas is finished, extract the sampling pipeline, the carrier gas gets into from the carrier gas pipeline and sweeps in order to clear away remaining flue gas to internal standard sample ration ring, sample ration ring and pipeline, switches first two-position tee bend solenoid valve state simultaneously, starts a cigarette suction module and extracts ambient air and sweeps the suction pipeline.
The results of an on-line analysis of total smoke (3 rd) from a commercially available heated cigarette using a gas chromatograph mass spectrometer (GC/MS) as an analytical detector are shown in fig. 5.
Example 2
Heated cigarette smoke mouth-by-mouth analysis
Example 1 was repeated according to the same procedure as described, with the sample quantification loop capturing the fumes port by port in the suction port order for on-line analysis.
Example 3
And (3) detecting gas-phase components of the smoke of the heated cigarette on line.
Example 1 was repeated according to the same procedure as described, with the addition of Cambridge filter in the tobacco holder, and the heated cigarette smoke gas phase was analyzed on-line.
Example 4
Example 1 was repeated according to the same procedure as described, but without the addition of an internal standard gas.
Example 5
Example 1 was repeated following the same procedure as described, but with the transfer line soak temperature set at 45 ℃.
Example 6
The example 1 is repeated according to the same steps, but the cigarette is not heated in the cigarette holder, the ambient air is directly extracted to enter a sample quantitative loop for analysis, a total ion flow diagram is obtained, the three components of nicotine, triacetin and glycerin can be detected through the data analysis of the total ion flow diagram, and the residual rates are 0.51%, 0.23% and 0.11% respectively.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The on-line analysis and detection device for the smoke of the heated cigarette is characterized by comprising a cigarette holder (100), a cigarette suction module (200), a sample quantification ring (302), an internal standard sample quantification ring (401), a ten-way valve (800), an on-line smoke analysis module (500), a flow path system and a control module;
the cigarette holder (100), the cigarette suction module (200), the sample quantification ring (302), the internal standard sample quantification ring (401) and the online smoke analysis module (500) are all communicated with the ten-way valve (800) through a flow path system, and the ten-way valve (800) is also used for being communicated with external carrier gas;
the cigarette holder (100), the cigarette suction module (200), the ten-way valve (800), the online smoke analysis module (500) and the flow path system are all controlled by the control module; wherein the content of the first and second substances,
the sample quantitative ring (302) is used for collecting a smoke sample and loading the smoke sample into the online smoke analysis module (500) through a carrier gas;
the internal standard sample quantitative ring (401) is used for collecting an internal standard gas sample and loading the internal standard gas sample into the online smoke analysis module (500) through a carrier gas;
the online smoke analysis module (500) is used for receiving the smoke sample and the internal standard gas sample to perform smoke online analysis and detection.
2. The on-line heated cigarette smoke analyzing and detecting device according to claim 1, wherein said flow path system comprises a flow regulating valve (705) and a plurality of pipelines;
when the ten-way valve (800) is in a first state, the cigarette holder (100), the sample quantifying ring (302) and the cigarette suction module (200) are sequentially connected through the ten-way valve (800) and a plurality of pipelines, the external internal standard gas, the internal standard sample quantifying ring (401) and the sampling pump are sequentially connected through the ten-way valve (800) and the plurality of pipelines, and the external carrier gas, the flow regulating valve (705) and the online smoke analysis module (500) are sequentially connected through the ten-way valve (800) and the plurality of pipelines;
when ten logical valve (800) are in the second state, hold cigarette ware (100), cigarette smoking module (200) and pass through ten logical valve (800) and a plurality of pipeline connect gradually, outside carrier gas, flow control valve (705), interior label sample ration ring (401), sample ration ring (302), online flue gas analysis module (500) pass through ten logical valve (800) and a plurality of pipeline connect gradually, and outside interior label gas, sampling pump pass through ten logical valve (800) and a plurality of pipeline connect gradually.
3. The on-line heated cigarette smoke analysis and detection device according to claim 1 or 2, further comprising a residual smoke absorption module (600), wherein said flow path system further comprises a first two-position three-way solenoid valve (703);
a first port (3-1) of the first two-position three-way electromagnetic valve (703) is communicated with the residual smoke absorption module (600), a second port (3-2) of the first two-position three-way electromagnetic valve (703) is communicated with the ten-way valve (800), and a third port (3-3) of the first two-position three-way electromagnetic valve (703) is communicated with the cigarette suction module (200);
when the first two-position three-way electromagnetic valve (703) is in a first state, the second port (3-2) is communicated with the third port (3-3), and when the first two-position three-way electromagnetic valve (703) is in a second state, the first port (3-1) is communicated with the third port (3-3).
4. The on-line heated cigarette smoke analyzing and detecting device according to claim 3, wherein said residual smoke absorbing module (600) comprises a sorbent tube (602) and a sorbent (601) filled therein, one end of said sorbent tube (602) is communicated with said first port (3-1), and the other end of said sorbent tube (602) is evacuated.
5. The on-line heated cigarette smoke analysis and detection device according to claim 4, wherein the adsorbent (601) is one or more of activated carbon, graphitized carbon black and molecular sieve, and polyethylene sieve plates are filled at two ends of the adsorbent (601).
6. The on-line heated cigarette smoke analysis and detection device according to claim 1 or 2, wherein the internal standard substance of the internal standard gas is one or more of ethanol, deuterated benzene, deuterated toluene, deuterated o-xylene and deuterated p-xylene, and the concentration of the internal standard gas is 1-500 ppm.
7. The heated cigarette smoke online analysis and detection device according to claim 1 or 2, wherein the online smoke analysis module (500) comprises one of a gas chromatograph, a gas chromatograph-mass spectrometer, an online mass spectrometer and an ion mobility spectrometer, and is further communicated with an external carrier gas; the cigarette suction module (200) comprises a suction needle cylinder (201) and a motor (203) for driving a piston (202) in the suction needle cylinder to reciprocate; the parameters of the cigarette suction module (200) are set as follows: the suction curve is one of a bell shape, a triangle and a rectangle, the suction capacity is 5-150mL, the suction duration is 0.8-10s, and the suction interval is 15-120 s; the volume of the sample quantitative ring (302) is 0.5-3mL, and the volume of the internal standard sample quantitative ring (401) is 0.25-1 mL.
8. The on-line heated cigarette smoke analysis and detection device according to claim 1 or 2, wherein the ten-way valve (800), the sample quantitative ring (302), the connecting pipeline between the cigarette holder (100) and the ten-way valve (800), the connecting pipeline between the cigarette smoking module (200) and the ten-way valve (800), and the connecting pipeline between the ten-way valve (800) and the on-line smoke analysis module (500) are all disposed in a heating and heat preservation box, and the heating and heat preservation temperature is 40-300 ℃.
9. An online analysis and detection method for the smoke of a heated cigarette, which is characterized by adopting the online analysis and detection device for the smoke of the heated cigarette as claimed in any one of claims 1 to 8 to carry out online analysis and detection, and comprises the following steps:
inserting the heated cigarette into a cigarette holder (100) and heating;
starting the cigarette suction module (200), and collecting a smoke sample with a preset volume by a sample quantitative ring (302) in the smoke suction process;
pumping the internal standard gas into an internal standard sample quantifying ring (401), and collecting an internal standard gas sample with a preset volume by the internal standard sample quantifying ring (401);
and loading the flue gas sample and the internal standard gas sample into an online flue gas analysis module (500) through carrier gas to perform online flue gas analysis and detection.
10. The heated cigarette smoke on-line analysis and detection method according to claim 11, further comprising:
when the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module (500) through the carrier gas, the smoke in the cigarette suction module (200) is discharged;
after the smoke sample and the internal standard gas sample are loaded into the online smoke analysis module (500), the online smoke analysis module (500) is disconnected from the flow path system, carrier gas is introduced to purge the sample quantification ring (302), the internal standard sample quantification ring (401), the ten-way valve (800), the pipeline between the ten-way valve (800) and the online smoke analysis module (500), and the cigarette suction module (200) is started to extract ambient air to purge the pipeline between the cigarette holder (100) and the ten-way valve (800) and the pipeline between the ten-way valve (800) and the cigarette suction module (200).
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