CN206696228U - A kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve - Google Patents

A kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve Download PDF

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CN206696228U
CN206696228U CN201720575482.2U CN201720575482U CN206696228U CN 206696228 U CN206696228 U CN 206696228U CN 201720575482 U CN201720575482 U CN 201720575482U CN 206696228 U CN206696228 U CN 206696228U
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flue gas
port
cigarette
photo
syringe
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胡永华
王健
田振峰
陈开波
徐迎波
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China Tobacco Anhui Industrial Co Ltd
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China Tobacco Anhui Industrial Co Ltd
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Abstract

The utility model discloses a kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve, it is characterized in that setting syringe, smoking machine, flue gas transmission quartz capillary and photo-ionisation time of-flight mass spectrometer;Front end of the syringe needle is provided with flue gas sampling port and flue gas input port;The suction cylinder with smoking machine, cigarette seizing device are connected respectively for first and second port of the three-way solenoid valve of smoking machine, and the 3rd port can both have been communicated by flue gas exit pipe road with air, can also be connected with the flue gas input port of syringe;One end of flue gas transmission quartz capillary is connected with the flue gas sampling port of syringe, and the other end enters in the vacuum ultraviolet ionized area of photo-ionisation time of-flight mass spectrometer.The utility model is simple in construction, easy to operate, it is suitable for the on-line measurement gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve under standard cigarettes puffing regimenses, so as to realize the function that standard is carried out to isomer in gaseous phase of main stream smoke of cigarette composition and is identified online.

Description

A kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve
Technical field
The utility model belongs to cigarette smoke chemical composition analysis technical field, and in particular to a kind of standard cigarettes aspirate mould The on-line measurement device of cigarette mainstream flue gas gas chemistry composition photo-ionisation efficiency curve under formula, so as to realize to cigarette main flue Isomer carries out the function that standard is identified online in gas gas phase composition.
Background technology
Cigarette smoke is a kind of complicated aerosol mixt being made up of thousands of kinds of chemical compositions.In order to study conveniently, Cigarette smoke is divided into people's generally use cambridge filter into gaseous substance and granule phase substance matter two parts are individually studied.Wherein, The proportion of amount of flue gas emission shared by gaseous substance is up to 92%, not only containing a variety of harmful components, and to the sense organ of cigarette smoke Quality also has highly important influence;In addition, gaseous substance property is active, the change of internal material composition is very fast.Therefore, it is The analysis result of flue gas situation in smoker oral cavity can be characterized by obtaining, in recent years to fresh single port components in cigarette smoke gas phase into Divide and carry out online and analyze and research in real time to be increasingly subject to the concern and attention of people.
The soft ionization mass-spectrometric technique such as ion-molecule reaction mass spectrum and vacuum laser ultraviolet light MALDI-MS, due to nothing The advantages that fragment, speed responsive are fast, high sensitivity and suitable multicomponent detect simultaneously, it has also become cigarette smoke is online and in real time point The effective means of analysis.However, in application this kind of soft ionization mass-spectrometric technique analysis cigarette smoke, still suffer from terms of two Problem:On the one hand, many chemical compositions all have isomer in cigarette smoke, and different with dividing with the increase of molecular weight The quantity of structure can increase rapidly;But what the ionization source energy of above-mentioned soft ionization mass-spectrometric technique was usually fixed, they can only give The soft ionization mass spectrogram gone out under fixed ionization source energy, and cannot be distinguished by isomer only according to mass spectrogram.It is another Aspect, due to can not be made a distinction to the isomer oxide precursor ion included in a soft ionization mass spectra peak, Thus also just it is difficult to carry out accurate quantitative analysis to single isomers.In order to solve the above problems, Eschner et al. (Eschner M S,Selmani I,Groger T M,et al.Online comprehensive two-dimensional characterization of puff-by-puff resolved cigarette smoke by hyphenation of fast gas chromatography to single-photon ionization time-of-flight mass spectrometry:quantification of hazardous volatile organic compounds.Anal Chem,2011,83(17):6619-6627.) once established the rare gas of a set of online fast gas chromatography series electrical beamlet pumping Body quasi-molecule ionizes light source flight time mass spectrum device, the isomer in flue gas composition is separated and quantitative analysis. Although the technology preferably improves the qualitative and quantitative analysis effect of isomer, due to by online quick gas phase color The limitation of separating capacity is composed, many isomers still can not be isolated and identified.
Synchrotron radiation VUV single-photon ionization ionization time of flight, it is not only able to survey under fixed photon energy The Photoionization Mass Spectrometry figure of test substance is measured, and there can also be the spy of wavelength continuously-tuning using synchrotron radiation vacuum-ultraviolet light Point, the photo-ionisation efficiency curve of different molecular weight chemical composition is obtained, isomerism in measurement of species is treated so as to realize Body is identified and compared.Wang Cheng brightness et al. (Wang Chenghui, Hu Yonghua, Wang Jian, waits the ionization energy meter of cigarette smoke chemical compositions Calculate and its scientific and technological using tobaccos in qualitative analysis, 2011,293 (12):26-33.) once utilize homemade manual cigarette cigarette Gas sampling syringe combination transmission synchrotron topography flight time mass spectrum measures first components in cigarette smoke gas phase chemical composition Photo-ionisation efficiency curve, and the ionization energy of material molecule is obtained according to " flex point " on curve, tentatively realize to cigarette smoke Isomeric identification in gas gas-phase objects.Pan et al. (Pan Y, Hu Y H, Wang J, et al.Online characterization of isomeric/isobaric components in the gas phase of mainstream cigarette smoke by tunable synchrotron radiation vacuum ultraviolet photoionization time-of-flight mass spectrometry and photoionization efficiency curve simulation.Analytical Chemistry,2013,85(24): Above-mentioned identical experimental provision and method 11993-12001.) are utilized, in combination with the simulation of photo-ionisation efficiency curve, is realized To the online accurate identification of isomer in components in cigarette smoke gas phase thing, and obtain in same mass spectra peak shared by different isomer Molar percentage.Although the studies above is established using photo-ionisation efficiency curve to same point in components in cigarette smoke gas phase composition The method that isomers carries out Qualitative Identification and quantitative analysis, but its experimental provision can only use manual mode smoking cigarette, it is difficult Cigarette is aspirated under the suction mode of standard with realizing;And international cigarette smoking mode, it is using commercialization What smoking machine was carried out under the suction mode of international standard, and under different suction modes, its smoke chemistry composition have compared with Big difference.Therefore, the photo-ionisation efficiency curve obtained using manual mode smoking cigarette, its qualitative and quantitative analysis result without Method carries out standard evaluation from the angle that smoke chemistry forms to cigarette quality.In addition, manual mode smoking cigarette, can not also be realized The photo-ionisation efficiency curve of different puff number flue gases is determined under the conditions of canonical parameter.So its concrete application receives very Big limitation.
Utility model content
The utility model is to avoid the weak point present in above-mentioned prior art, there is provided a kind of simple in construction, operation side Just, can realize using commercial smoking machine under the suction mode of international standard, on-line measurement gaseous phase of main stream smoke of cigarette composition The measurement apparatus of photo-ionisation efficiency curve, so as to be same in tobacco scientific and technical personnel's on-line analysis gaseous phase of main stream smoke of cigarette composition Enantiomers provide a kind of good technological means.
The utility model solves technical problem and adopted the following technical scheme that:
A kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve, it is structurally characterized in that:Note is set Emitter, commercial single channel smoking machine, flue gas transmission quartz capillary and photo-ionisation time of-flight mass spectrometer;Fly in the photo-ionisation The outside of row time mass spectrum instrument is provided with top vacuum pumping opening and lower vacuum bleeding point, is internally provided with vacuum ultraviolet light source With vacuum ultraviolet ionized area;
The front end of the syringe is provided with two ports, wherein a port is to pass through two-port valve a and the flue gas The connected flue gas sampling port of quartz capillary is transmitted, second port is what is be connected by two-port valve b with flue gas input channel Flue gas input port;
The front end of the suction cylinder of the commercial single channel smoking machine is provided with three-way solenoid valve;The of the three-way solenoid valve Single port is connected with the suction cylinder of the commercial single channel smoking machine, second port and the cigarette seizing device of pluggable Cigarette It is connected, the 3rd port is connected with flue gas exit pipe road, and the flue gas exit pipe road can both communicate with atmospheric environment, can also It is connected with the flue gas input channel of the syringe;
One end of the flue gas transmission quartz capillary is connected with the flue gas sampling port of the syringe, and the other end passes through The cavity wall of the photo-ionisation time of-flight mass spectrometer enters in the vacuum ultraviolet ionized area.
Compared with the prior art, the beneficial effects of the utility model are embodied in:
1st, the utility model is simple in construction, easy to operate, without carrying out any transformation to commercial single channel smoking machine In the case of, it is possible to achieve under the suction mode of international standard, the photo-ionisation effect of on-line measurement gaseous phase of main stream smoke of cigarette composition Rate curve, so as to smoke chemistry composition, the online identification of isomer especially therein and quantitative comparison, can Stable analysis result is obtained, the angle be advantageous to from smoke chemistry composition carries out standard evaluation to cigarette quality.
2nd, the utility model is not only able to measure first gaseous phase of main stream smoke of cigarette composition under the suction mode of standard Photo-ionisation efficiency curve, and the photo-ionisation efficiency that can also easily measure flue gas gas phase composition under other puff numbers is bent Line.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model;
Fig. 2 be the first gaseous phase of main stream smoke of cigarette thing of embodiment 1 in mass number be respectively 44,58,70 and 72 it is several The photo-ionisation efficiency curve of flue gas composition.
Fig. 3 be 2 second mouthfuls of gaseous phase of main stream smoke of cigarette things of embodiment in mass number be respectively 44,58,70 and 72 it is several The photo-ionisation efficiency curve of flue gas composition.
Label in figure:1 syringe, 2 flue gas sampling ports, 3 two-port valve a, 4 flue gas input ports, 5 two-port valve b, 6 flue gases Input channel, 7 commercial single channel smoking machines, 8 suction cylinders, 9 three-way solenoid valves, 10 cigarette seizing devices, 11 Cigarettes, 12 flue gases Output channel, 13 flue gases transmission quartz capillary, 14 photo-ionisation time of-flight mass spectrometers, 15 top vacuum pumping openings, 16 bottoms Vacuum pumping opening, 17 vacuum ultraviolet light sources, 18 vacuum ultraviolet ionized areas.
Embodiment
The utility model is further illustrated below by way of embodiment, and with reference to accompanying drawing.
As shown in figure 1, each constituting portion of device point includes:Syringe 1, commercial single channel smoking machine 7, flue gas transmission quartz Capillary 13 and photo-ionisation time of-flight mass spectrometer 14;The outside of photo-ionisation time of-flight mass spectrometer 14 is provided with top vacuum Bleeding point 15 and lower vacuum bleeding point 16, it is internally provided with vacuum ultraviolet light source 17 and vacuum ultraviolet ionized area 18;
The front end of syringe 1 is provided with two ports, wherein a port is to transmit stone by two-port valve a 3 and flue gas The connected flue gas sampling port 2 of English capillary 13, second port are what is be connected by two-port valve b 5 with flue gas input channel 6 Flue gas input port 4;
The front end of the suction cylinder 8 of commercial single channel smoking machine 7 is provided with three-way solenoid valve 9;The first end of three-way solenoid valve 9 Mouth is connected with the suction cylinder 8 of commercial single channel smoking machine 7, second port and the phase of cigarette seizing device 10 of pluggable Cigarette 11 Even, the 3rd port is connected with flue gas exit pipe road 12, and flue gas exit pipe road 12 can both communicate with atmospheric environment, can also be with The flue gas input channel 6 of syringe 1 is connected;
One end of flue gas transmission quartz capillary 13 is connected with the flue gas sampling port 2 of syringe 1, and the other end passes through photoelectricity Cavity wall from time of-flight mass spectrometer 14 enters in vacuum ultraviolet ionized area 18.
Single channel smoking machine 7 used in the utility model embodiment is given birth to for German BORGWALDT KC GMBH companies The LM1 type single channel smoking machines of production;Used photo-ionisation time of-flight mass spectrometer 14 is that cigarette industry Limited Liability is public in Anhui Department and the instrument of China Science & Technology University's NSRL joint research and development, its vacuum ultraviolet light source 17 both can be Vacuum UV lamp or synchrotron radiation vacuum-ultraviolet light.
In specific implementation, syringe 1 aspirates drum outer wall and flue gas transmission quartz capillary 13 is located at the flue gas of syringe 1 Part between sample port 2 and the cavity wall of vacuum ultraviolet ionized area 18 of photo-ionisation time of-flight mass spectrometer 14 is provided with electricity and added The torrid zone, heating-up temperature are set and controlled by a special temperature controller;Flue gas exit pipe road 12 and flue gas input channel 6 it Between be attached using transition conduit, in addition, can also gastight any quick-release mode be attached.
Before experiment, the working power of photo-ionisation time of-flight mass spectrometer 14 and commercial single channel smoking machine 7 is first turned on;If Put the smoking parameters condition of commercial single channel smoking machine 7;Set syringe 1 and aspirate drum outer wall and flue gas transmission quartz capillary 13 Heating-up temperature;Then cambridge filter is loaded in cigarette clamper 10.Treat photo-ionisation time of-flight mass spectrometer 14 vacuum, And syringe 1 aspirates drum outer wall and the heating-up temperature of flue gas transmission quartz capillary 13 meets when requiring, you can is tested.
In experimentation, when determining the photo-ionisation efficiency curve of first gaseous phase of main stream smoke of cigarette composition, connect first Cigarette receiving gas output channel 12 and flue gas input channel 6, open two-port valve b, close two-port valve a;Then Cigarette 11 is inserted In cigarette clamper 10, igniting suction.When gaseous phase of main stream smoke of cigarette thing is pushed into syringe 1 by commercial single channel smoking machine 7 Afterwards, stop the suction of commercial single channel smoking machine 7, and close two-port valve b, open two-port valve a;At the same time, light is started immediately Ionization time-of-flight mass spectrometer 14 measures to flue gas.
When needing to measure the photo-ionisation efficiency curve of other puff number gaseous phase of main stream smoke of cigarette compositions, first by cigarette Gas output channel 12 and flue gas input channel 6 disconnect, and open two-port valve b, close two-port valve a, and multiple aspirating syringe 1 is with general Residual flue gas in it is removed clean;Then Cigarette 11 is inserted in cigarette clamper 10, igniting suction;When first cigarette After gas suction terminates, the Cigarette 11 of burning is removed, allows commercial single channel smoking machine 7 to carry out suction several times, to remove suction and pumping The residual flue gas of cylinder 8 and flue gas exit pipe road 12;And then, the Cigarette 11 of burning is reinserted into cigarette clamper 10 In, carry out lower a bite flue gas suction.When needing to measure the photo-ionisation efficiency curve of certain mouthful of flue gas, after in last time, suction terminated, Flue gas exit pipe road 12 is connected with flue gas input channel 6, after completing suction, you can realize to this mouthful of cigarette mainstream flue gas gas The measurement of the photo-ionisation efficiency curve of phase constituent.
Embodiment 1
(i.e. every mouthful suction 35mL, is aspirated 2 seconds, and suction gap is 58 seconds) the measurement first under standard aspiration pattern The photo-ionisation efficiency curve of components in cigarette smoke gas phase chemical composition.Photo-ionisation time of-flight mass spectrometer uses synchrotron radiation VUV Light makees ionization light source, and its energy scan scope is 8.0~10.6eV;Suction drum outer wall and flue gas the transmission quartz wool of syringe The heating-up temperature of tubule is set as 200 DEG C.
Mass number is respectively 44,58,70 and 72 several light for representing type flue gas composition in gaseous phase of main stream smoke of cigarette thing Ionization efficiency curve, referring to Fig. 2.
Embodiment 2
Substantially with embodiment 1, except that what is measured under standard aspiration pattern is second mouthful of cigarette mainstream flue gas gas The photo-ionisation efficiency curve of phase chemical composition.Now, the smoking parameters condition of smoking machine is set as every mouthful of suction 35mL, suction 2 seconds, suction gap be 10 seconds, therefore, the suction of second mouthful of cigarette smoke is the smoking after the suction of first flue gas terminates Machine is carried out continuously what is carried out on the basis of four suctions.
Mass number is respectively 44,58,70 and 72 several light for representing type flue gas composition in gaseous phase of main stream smoke of cigarette thing Ionization efficiency curve, referring to Fig. 3.
To sum up, the measurement dress of a kind of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve provided by the utility model Put, can not only realize that the photo-ionisation efficiency that first components in cigarette smoke gas phase chemical composition is measured under standard aspiration pattern is bent Line, and the photo-ionisation efficiency curve of flue gas gas phase composition under other puff numbers can also be easily measured, so as to be tobacco section The isomer that skill personnel are accurate, scientifically analyze in gaseous phase of main stream smoke of cigarette composition provides a kind of effective technical side Method and means.
Exemplary embodiment of the present utility model is these are only, it is all in this reality not to limit the utility model With all any modification, equivalent and improvement made within new spirit and principle etc., should be included in of the present utility model Within protection domain.

Claims (2)

1. a kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve, it is characterized in that:Syringe is set (1), commercial single channel smoking machine (7), flue gas transmission quartz capillary (13) and photo-ionisation time of-flight mass spectrometer (14);
The outside of the photo-ionisation time of-flight mass spectrometer (14) is provided with top vacuum pumping opening (15) and lower vacuum is taken out Gas port (16), it is internally provided with vacuum ultraviolet light source (17) and vacuum ultraviolet ionized area (18);
The front end of the syringe (1) is provided with two ports, wherein a port is to pass through two-port valve a (3) and the cigarette The connected flue gas sampling port (2) of gas transmission quartz capillary (13), second port are defeated by two-port valve b (5) and flue gas Enter the connected flue gas input port (4) of pipeline (6);
The front end of the suction cylinder (8) of the commercial single channel smoking machine (7) is provided with three-way solenoid valve (9);The electromagnetic three-way The first port of valve (9) is connected with the suction cylinder (8) of the commercial single channel smoking machine (7), second port and pluggable cigarette The cigarette seizing device (10) of cigarette (11) is connected, and the 3rd port is connected with flue gas exit pipe road (12), and the flue gas exit pipe Road (12) can both communicate with atmospheric environment, can also be connected with the flue gas input channel (6) of the syringe (1);
One end of the flue gas transmission quartz capillary (13) is connected with the flue gas sampling port (2) of the syringe (1), another The cavity wall through the photo-ionisation time of-flight mass spectrometer (14) is held to enter in the vacuum ultraviolet ionized area (18).
2. a kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve according to claim 1, its It is characterized in:Drum outer wall is aspirated in syringe (1) and flue gas transmission quartz capillary (13) is located at the flue gas sampling of syringe (1) Part between port (2) and vacuum ultraviolet ionized area (18) cavity wall of photo-ionisation time of-flight mass spectrometer (14) is provided with electricity Heating tape.
CN201720575482.2U 2017-05-23 2017-05-23 A kind of measurement apparatus of gaseous phase of main stream smoke of cigarette composition photo-ionisation efficiency curve Active CN206696228U (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110186996A (en) * 2019-07-15 2019-08-30 安徽中烟工业有限责任公司 A kind of cigarette glows the on-line measurement device of side-stream smoke gas phase composition photo-ionisation efficiency curve
CN110608985A (en) * 2019-09-09 2019-12-24 河南中烟工业有限责任公司 Dynamic filter ventilation rate detection device based on suction mode
CN110967394A (en) * 2019-07-26 2020-04-07 安徽中烟工业有限责任公司 Method for identifying cigarette smoke gas phase component isomerides
CN112858450A (en) * 2021-01-18 2021-05-28 中国烟草总公司郑州烟草研究院 Cigarette smoke online collecting and ionizing device and method
CN113295758A (en) * 2021-05-21 2021-08-24 中国科学院合肥物质科学研究院 Mass spectrometer for on-line detection of chemical components in aerosol particles of cigarette smoke
CN113702484A (en) * 2021-07-19 2021-11-26 知健生物分子研究院(南京)有限公司 Cigarette smoke gas phase component analysis method based on DART-MS

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110186996A (en) * 2019-07-15 2019-08-30 安徽中烟工业有限责任公司 A kind of cigarette glows the on-line measurement device of side-stream smoke gas phase composition photo-ionisation efficiency curve
CN110186996B (en) * 2019-07-15 2024-02-13 安徽中烟工业有限责任公司 Online measurement device for photoelectric efficiency curve of gas phase component of smoldering side stream smoke of cigarette
CN110967394A (en) * 2019-07-26 2020-04-07 安徽中烟工业有限责任公司 Method for identifying cigarette smoke gas phase component isomerides
CN110967394B (en) * 2019-07-26 2022-06-14 安徽中烟工业有限责任公司 Method for identifying cigarette smoke gas phase component isomerides
CN110608985A (en) * 2019-09-09 2019-12-24 河南中烟工业有限责任公司 Dynamic filter ventilation rate detection device based on suction mode
CN112858450A (en) * 2021-01-18 2021-05-28 中国烟草总公司郑州烟草研究院 Cigarette smoke online collecting and ionizing device and method
CN113295758A (en) * 2021-05-21 2021-08-24 中国科学院合肥物质科学研究院 Mass spectrometer for on-line detection of chemical components in aerosol particles of cigarette smoke
CN113702484A (en) * 2021-07-19 2021-11-26 知健生物分子研究院(南京)有限公司 Cigarette smoke gas phase component analysis method based on DART-MS

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