CN112858450A - Cigarette smoke online collecting and ionizing device and method - Google Patents
Cigarette smoke online collecting and ionizing device and method Download PDFInfo
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- CN112858450A CN112858450A CN202110062680.XA CN202110062680A CN112858450A CN 112858450 A CN112858450 A CN 112858450A CN 202110062680 A CN202110062680 A CN 202110062680A CN 112858450 A CN112858450 A CN 112858450A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
A cigarette smoke online acquisition ionization device and a method thereof are provided, the cigarette smoke online acquisition ionization device comprises a cigarette holder, a suction module, a suction gas path, a sampling gas path, an ionization cavity and an ionization module, wherein the cigarette holder is communicated with the suction module through the suction gas path; the sampling gas circuit is communicated with the suction gas circuit, and the ionization module is communicated with the sampling gas circuit through the ionization cavity. The invention realizes the on-line collection of fresh smoke; the collection and ionization processes of the smoke are organically integrated and carried out simultaneously, and a powerful tool is provided for real-time online analysis of the smoke of the cigarette; through the design of a plurality of components between the suction gas path and the sampling gas path, the suction capacity of the suction module is not influenced while the smoke is collected, the accuracy and the stability of the port-by-port suction can be ensured, and the sample introduction and the ionization stability of the ionization cavity can be ensured; the device has strong universality and can be adapted to various instruments or equipment for separation and analysis based on the ion state.
Description
Technical Field
The invention relates to the field of cigarette smoke analysis, in particular to an online cigarette smoke collection and ionization device and method.
Background
The cigarette smoke is the most direct object for consumers to consume cigarette commodities, and the quality of the cigarette smoke is an important factor for determining the quality of the cigarette commodities. The method has important significance for enhancing the analysis of cigarette smoke, analyzing the quality of cigarettes and guiding the technical formula, processing and research and development of new products of the cigarettes.
The current common cigarette smoke analysis standard analysis method is based on off-line analysis, and the specific implementation mode is generally as follows: the method comprises the steps of collecting a particulate phase part and a gas phase part of cigarette smoke respectively by utilizing a glass fiber filter and an absorption liquid or a trap, obtaining a proper analysis test solution by a certain sample pretreatment means, and finally carrying out qualitative and quantitative analysis by conventional analysis technologies such as GC, LC, GC-MS, LC-MS and the like. The formation of cigarette smoke is a dynamic process, the off-line analysis treatment time is long, the smoke can be aged, other substances are easily introduced artificially in the sample pretreatment process, and the real chemical characteristics of the smoke cannot be reflected.
With the development of the soft ionization mass spectrometry technology, the on-line analysis research of cigarette smoke is favored by researchers. The conventional cigarette smoke online analysis device and method are generally established on the basis of the combination of a smoking machine and online analysis mass spectrometry: the patent (CN102192950A) discloses an on-line analysis device for gas-phase chemical components in cigarette smoke, which is characterized in that a smoke transmission quartz capillary tube is arranged between a suction tube and an on-line analysis mass spectrometer of a commercial smoking machine; the patent (CN103364484A) discloses a cigarette mainstream smoke online analysis device and method, the device comprises a smoking machine and an atmospheric pressure chemical ionization tandem mass spectrometer, a mainstream smoke collection bottle is arranged between the smoking machine and the atmospheric pressure chemical ionization tandem mass spectrometer, the online analysis method is that after the cigarette is smoked, the mainstream smoke is collected and enters the mainstream smoke collection bottle, and a smoke sample is directly introduced into an atmospheric pressure chemical ionization tandem mass spectrometer ion source through a sample introduction valve for rapid analysis. Although the online analysis of the cigarette smoke is realized by the two patents, the accuracy of the smoking machine smoking capacity and the quantitative accuracy of the smoke mass spectrometry cannot be considered, the reason is that the mass spectrometry has a vacuum system of the mass spectrometry, no matter the mass spectrometry passes through a quartz capillary tube or a smoke collection bottle, the mass spectrometry has a constant smoking flow, and the accuracy of the smoking machine smoking capacity cannot be influenced by the constant smoking flow without gas compensation. On the other hand, the accuracy of mass spectrometry is determined by the sampling stability, and the change of the internal and external air pressure of the mass spectrometry sampling port can be caused in the smoking machine suction process, and the air pressure change can influence the stability of the mass spectrometry sampling amount to a certain extent.
Disclosure of Invention
In order to solve the problems, the invention provides an on-line cigarette smoke collecting and ionizing device and method.
The cigarette smoke online acquisition ionization device comprises a cigarette holder, a suction module, a suction gas path, a sampling gas path, an ionization cavity and an ionization module, wherein the cigarette holder is communicated with the suction module through the suction gas path; the sampling gas circuit is communicated with the suction gas circuit, and the ionization module is communicated with the sampling gas circuit through the ionization cavity. When the suction module starts suction, the electromagnetic valve is opened, and the suction gas path is communicated; and after the suction module finishes one suction action, the electromagnetic valve is immediately closed, and the suction air channel is disconnected.
The suction air path is communicated with the sampling air path through a four-way valve.
The cigarette holder is communicated with the electromagnetic valve and communicated with the suction module through the four-way valve.
The sampling gas circuit comprises a sampling pump (6) and a flow controller (5), the upstream end of the sampling pump (6) is communicated with the flow controller (5) through a four-way valve (3), and the downstream end of the sampling pump (6) is communicated with the ionization chamber.
The ionization chamber comprises a first interface, a second interface, a condensed liquid discharge port and a gas-phase ion outlet, wherein the first interface is communicated with the sampling pump; the second interface is communicated with the ionization module, and the gas-phase ion outlet is connected with the sample inlet of the analyzer.
Alternatively, the ionization module includes, but is not limited to, electrospray ionization, photoionization, PTR (proton transfer) ionization, LTP (low temperature plasma) ionization, and the like.
The sampling pump linearly adjusts the sampling flow, the adjusting range is 0-10 mL/s, and the flow adjusting precision is preferably 0.1 mL/s.
The flow controller controls the flow of the compensation gas, the control range of the flow controller is matched with the sampling flow of the sampling pump, the adjusting range of the flow controller is 0-10 mL/s, and the flow control precision is preferably 0.1 mL/s. The compensation gas includes, but is not limited to, air, nitrogen, helium, and the like, preferably nitrogen.
A method for on-line collection of an ionization device from cigarette smoke, the method comprising:
step A: turning on an ionization module;
and B: starting the flow controller and the sampling pump, and respectively adjusting the sampling flow of the sampling pump and the control flow of the flow controller to be consistent with each other so as to ensure that no pressure difference exists in the whole sampling gas circuit;
and C: setting a pumping program for the pumping module, the pumping program including but not limited to: pumping pattern (e.g., bell curve, step curve, etc.), pumping time, pumping cycle, and number of pumping ports; (ii) a
Step D: securing a smoking article (including but not limited to a cigarette, a heated cigarette, an electronic cigarette) to a cigarette holder, igniting or starting the smoking article
Step E: starting the suction module, controlling the electromagnetic valve to be opened by the suction module at the same time, connecting a suction gas path, controlling the electromagnetic valve to be immediately closed by the suction module after the suction module finishes one suction action, and disconnecting the suction gas path; during the suction period of the suction module, the flow controller and the sampling pump maintain constant flow speed operation, and the on-line collection of the smoke during the suction period is completed and the smoke is sent into the ionization chamber; the ionization module maintains operation, realizes the ionization of analyte in the flue gas.
Step F: and E, circulating the number of the suction ports set in the steps E to C to finish the real-time collection and ionization of the smoke in the whole suction program.
The invention provides an on-line cigarette smoke collecting and ionizing device and method. The on-line collection of fresh smoke is realized; the collection and ionization processes of the smoke are organically integrated and carried out simultaneously, and a powerful tool is provided for real-time online analysis of the smoke of the cigarette; through the design of a plurality of components between the suction gas path and the sampling gas path, the suction capacity of the suction module is not influenced while the smoke is collected, the accuracy and the stability of the port-by-port suction can be ensured, and the sample introduction and the ionization stability of the ionization cavity can be ensured; the device has strong universality and can be adapted to various instruments or equipment for separation and analysis based on the ion state.
Drawings
FIG. 1 is a schematic view of an on-line cigarette smoke collection and ionization device.
FIG. 2 is a schematic diagram of an electrospray ionization apparatus.
Fig. 3 is a schematic structural view of a cigarette smoke on-line collecting ionization device with an ionization module as an electrospray ionization device.
FIG. 4 is a graph of continuous monitoring of the release of glycerin and nicotine with smoking in a heated cigarette obtained by an on-line cigarette smoke collection and ionization device.
Detailed Description
The invention provides an on-line cigarette smoke collecting and ionizing device and a method thereof, which are described in detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1-3, an on-line cigarette smoke collecting and ionizing device and method includes a cigarette holder 1, a suction module 4, a suction gas path, a sampling gas path, an ionization chamber 7 and an ionization module 8, wherein the cigarette holder 1 is communicated with the suction module 4 through the suction gas path; the sampling gas circuit is communicated with the suction gas circuit, and the ionization module 8 is communicated with the sampling gas circuit through the ionization cavity 7. When the suction module starts suction, the electromagnetic valve is opened, and the suction gas path is communicated; and after the suction module finishes one suction action, the electromagnetic valve is immediately closed, and the suction air channel is disconnected.
And the suction gas path is communicated with the sampling gas path through a four-way valve.
The suction gas path comprises an electromagnetic valve, and the cigarette holder is communicated with the electromagnetic valve and is communicated with the suction module through a four-way valve.
The sampling gas circuit comprises a sampling pump (6) and a flow controller (5), the upstream end of the sampling pump (6) is communicated with the flow controller (5) through a four-way valve (3), and the downstream end of the sampling pump (6) is communicated with the ionization chamber.
The ionization chamber 7 comprises a first interface 71, a second interface 72, a condensed liquid discharge port 74 and a gas-phase ion outlet 73, wherein the first interface 71 is communicated with the sampling pump 6; the second interface 72 is communicated with the ionization module (8), and the gas-phase ion outlet 73 is connected with a sample inlet of the analysis instrument.
The ionization module 8 includes, but is not limited to, electrospray ionization, photoionization, PTR (proton transfer) ionization, LTP (low temperature plasma) ionization, and the like.
The sampling pump 6 linearly adjusts the sampling flow, and the adjusting range is 0-10 mL/s. The flow rate adjustment accuracy is preferably 0.1 mL/s.
The flow controller 5 controls the flow of the compensation gas, the control range of the flow controller is matched with the sampling flow of the sampling pump, and the adjusting range of the flow controller is 0-10 mL/s. The adjusting range is 0-10 mL/s, and the flow control precision is preferably 0.1 mL/s. The compensation gas includes, but is not limited to, air, nitrogen, helium, and the like, preferably nitrogen.
A method for on-line collection of an ionization device from cigarette smoke, the method comprising:
step A: turning on an ionization module;
and B: starting the flow controller and the sampling pump, and respectively adjusting the sampling flow of the sampling pump and the control flow of the flow controller to be consistent with each other so as to ensure that no pressure difference exists in the whole sampling gas circuit;
and C: setting a pumping program for the pumping module, the pumping program including but not limited to: pumping pattern (e.g., bell curve, step curve, etc.), pumping time, pumping cycle, and number of pumping ports;
step D: securing a tobacco product (including but not limited to a cigarette, a heated cigarette, an electronic cigarette) to a cigarette holder, igniting or starting the tobacco product;
step E: starting the suction module, controlling the electromagnetic valve to be opened by the suction module at the same time, connecting a suction gas path, controlling the electromagnetic valve to be immediately closed by the suction module after the suction module finishes one suction action, and disconnecting the suction gas path; during the suction period of the suction module, the flow controller and the sampling pump maintain constant flow speed operation, and the on-line collection of the smoke during the suction period is completed and the smoke is sent into the ionization chamber; the ionization module maintains operation, realizes the ionization of analyte in the flue gas.
Step F: and E, circulating the number of the suction ports set in the steps E to C to finish the real-time collection and ionization of the smoke in the whole suction program.
Examples
As shown in fig. 3, the ionization module 8 is configured as an electrospray ionization device, the electrospray ionization device includes a sheath gas shell 81, a sheath gas inlet 83 is disposed on the sheath gas shell 81, one end of a quartz capillary 82 is disposed inside the sheath gas shell 81, the other end of the quartz capillary 82 is communicated with a solvent 84, a voltage 85 (preferably 3-5 kV) is applied to the quartz capillary 82, and the sheath gas shell 81 is in sealed communication with the ionization chamber 7. A sheath gas, preferably nitrogen, is introduced at a flow rate from the sheath gas inlet 83. A switch valve can be arranged at a condensed liquid discharge port of the ionization chamber, and the opening and closing of the switch valve are controlled according to actual requirements.
Figure 4 shows a graph of the continuous monitoring of the release of glycerol and nicotine with the smoking process in a heated cigarette obtained by an on-line cigarette smoke collection ionization device. Wherein the pumping volume is 55mL, the pumping time is 2s, the pumping period is 60s, the compensation gas is nitrogen, the flow of the compensation gas circuit is 10mL/s, the electrospray high pressure is 4000V, the electrospray solvent is methanol, and the state of the switch valve is open.
As an important component of online mass spectrometry, the quality of ionization source performance directly determines the accuracy of flue gas analysis and the sensitivity of an instrument. The invention organically integrates the cigarette smoke on-line extraction and ionization processes, ensures that the smoke is collected without influencing the suction capacity of a suction module through the design of a plurality of components between a suction gas path and a sampling gas path, can ensure the accuracy and stability of mouth-to-mouth suction, can also ensure the stability of sample introduction and ionization of an ionization cavity, can be suitable for various detection instruments (such as mass spectrums, ion chromatographs and the like) based on the analysis of the ionic state of the analyte, and has wide application prospect in the field of cigarette smoke analysis.
Finally, it should be noted that the above examples are only intended to describe the technical solutions of the present invention and not to limit the technical methods, the present invention can be extended in application to other modifications, variations, applications and embodiments, and therefore all such modifications, variations, applications, embodiments are considered to be within the spirit and teaching scope of the present invention.
Claims (9)
1. The cigarette smoke online acquisition ionization device comprises a cigarette holder (1), a suction module (4), a suction gas path, a sampling gas path, an ionization cavity (7) and an ionization module (8), and is characterized in that the cigarette holder (1) is communicated with the suction module (4) through the suction gas path; the sampling gas circuit is communicated with the suction gas circuit, and the ionization module (8) is communicated with the sampling gas circuit through the ionization cavity (7).
2. The cigarette smoke online collecting and ionizing device according to claim 1, wherein the suction gas path is communicated with the sampling gas path through a four-way valve (3).
3. The cigarette smoke online collecting and ionizing device according to claim 1, wherein the suction gas path comprises an electromagnetic valve (2), and the cigarette holder (1) is communicated with the electromagnetic valve (2) and communicated with the suction module (4) through a four-way valve (3).
4. The cigarette smoke online collecting and ionizing device according to claim 1, wherein the sampling gas circuit comprises a sampling pump (6) and a flow controller (5), the upstream end of the sampling pump (6) is communicated with the flow controller (5) through a four-way valve (3), and the downstream end of the sampling pump (6) is communicated with an ionizing cavity (7).
5. The cigarette smoke online collecting and ionizing device according to claim 1 or 4, wherein the ionizing chamber (7) comprises a first interface (71), a second interface (72), a condensed liquid discharge port (74) and a gas phase ion outlet (73), wherein the first interface (71) is communicated with the sampling pump (6); the second interface (72) is communicated with the ionization module (8), and the gas-phase ion outlet (73) is connected with a sample inlet of an analysis instrument.
6. The cigarette smoke online collecting and ionizing device of claim 1, wherein said ionizing module (8) comprises but is not limited to an electrospray ionization device, a photoionization device, a PTR (proton transfer) ionization device, an LTP (low temperature plasma) ionization device and the like.
7. The on-line cigarette smoke collecting and ionizing device according to claim 4, wherein the sampling pump (6) linearly adjusts the sampling flow, and the adjustment range is 0-10 mL/s.
8. The on-line cigarette smoke collecting and ionizing device according to claim 3, wherein the flow controller (5) controls the flow of the compensating gas, the control range of the flow controller is matched with the sampling flow of the sampling pump, and the adjusting range of the flow controller is 0-10 mL/s.
9. The method for on-line collection and ionization of cigarette smoke according to claim 1, wherein the method comprises the following steps:
step A: turning on an ionization module;
and B: starting the flow controller and the sampling pump, and respectively adjusting the sampling flow of the sampling pump and the control flow of the flow controller to be consistent with each other so as to ensure that no pressure difference exists in the whole sampling gas circuit;
and C: setting a pumping program for the pumping module, the pumping program including but not limited to: suction mode, suction time, suction cycle and suction port number;
step D: securing a tobacco product (including but not limited to a cigarette, a heated cigarette, an electronic cigarette) to a cigarette holder, igniting or starting the tobacco product;
step E: starting the suction module, controlling the electromagnetic valve to be opened by the suction module at the same time, connecting a suction gas path, controlling the electromagnetic valve to be immediately closed by the suction module after the suction module finishes one suction action, and disconnecting the suction gas path; during the suction period of the suction module, the flow controller and the sampling pump maintain constant flow speed operation, and the on-line collection of the smoke during the suction period is completed and the smoke is sent into the ionization chamber; the ionization module keeps running to realize ionization of the analyte in the smoke;
step F: and E, circulating the number of the suction ports set in the steps E to C to finish the real-time collection and ionization of the smoke in the whole suction program.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113431930A (en) * | 2021-06-30 | 2021-09-24 | 蜂巢能源科技有限公司 | Multi-way valve and collection device with same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113431930A (en) * | 2021-06-30 | 2021-09-24 | 蜂巢能源科技有限公司 | Multi-way valve and collection device with same |
| CN113431930B (en) * | 2021-06-30 | 2023-05-23 | 蜂巢能源科技有限公司 | Multi-way valve and collection device with same |
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