CN105467025A - Low-temperature cigarette smoke composition analysis method - Google Patents
Low-temperature cigarette smoke composition analysis method Download PDFInfo
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- CN105467025A CN105467025A CN201510788851.1A CN201510788851A CN105467025A CN 105467025 A CN105467025 A CN 105467025A CN 201510788851 A CN201510788851 A CN 201510788851A CN 105467025 A CN105467025 A CN 105467025A
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- G—PHYSICS
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- 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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- 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
- 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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- G01N30/6052—Construction of the column body
- G01N30/6073—Construction of the column body in open tubular form
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Abstract
The invention discloses a low-temperature cigarette smoke composition analysis method. The analysis method is as below: heating and splitting low temperature cigarette cut tobacco or sheets in an air environment at the temperature of 145-250 DEG C for 2-4 s; sending the smoke after splitting into a gas chromatography-mass spectrometer for component analysis; and then processing the test data to obtain the relative percentage of each component in the smoke. The present invention utilizes sophisticated thermal cracking technique to simulate the heating process of low temperature cigarette, and the gas chromatography-mass spectrometer analysis method is used to analyze the components in the low temperature cigarette smoke, so as to obtain the components and relative percentage of each component in the low temperature cigarette smoke, and obtain the change of smoke content in the smoking process of the low temperature cigarette. The method provides important references for the analysis of low temperature cigarette smoke and product development.
Description
Technical field
The present invention relates to a kind of low temperature cigarette fume component analysis method, belong to fume component analysis technical field.
Background technology
Low temperature cigarette is the incombustible cigarette of a kind of heating, low temperature cigarette utilizes special thermal source to heat (less than 500 degree even lower) pipe tobacco, pipe tobacco only heats and does not burn, pipe tobacco temperature is far below traditional cigarette, thus flue gas harmful chemical component and bio-toxicity significantly reduce, be the tobacco product closest to cigarette, belong to tobacco product category.At present, low temperature cigarette product is in development, although You Jijia tobacco company has developed low temperature cigarette product, product technology condition also needs Improvement and perfection.
By investigation foreign market on low temperature cigarette product, heating part, based on the hollow pen-like device of Cigarette size, is separated with by heating part by low temperature cigarette, by heating part and common cigarette similar.Flue gas analysis for this type of low temperature cigarette there is not yet bibliographical information in this respect.By consulting the documents and materials relevant to low temperature cigarette, have no patent and the document of the detection of low temperature cigarette smoke components.
Summary of the invention
The technical matters that the present invention solves provides a kind of and can analyze the method detecting low temperature cigarette smoke components relative content, may be used for the exploitation instructing tobacco company to low temperature cigarette.
Technical scheme of the present invention is, provides a kind of low temperature cigarette fume component analysis method, gets low temperature cigarette pipe tobacco or thin slice, and under air ambient, cracking is carried out in heating, and the temperature of described cracking is 145-250 DEG C, and the time of cracking is 2-4 second; Flue gas after cracking is input to gas chromatograph-mass spectrometer (GCMS) and carries out constituent analysis, then carry out test data processing the percentage contents that can obtain each material in flue gas.
Further, described cracking is carried out 8-12 time under same cracking temperature, and the time of each cracking is 2-4 second, the flue gas after each cracking is input to gas chromatograph-mass spectrometer (GCMS) and carries out constituent analysis.
Further, described cracking temperature is selected from following temperature range 145-155 DEG C, 190-200 DEG C and 240-250 DEG C.
Further, multiple cracking temperature is selected to carry out cracking respectively.
Further, described cracking temperature selects following three temperature spots: 150 DEG C, 195 DEG C and 246 DEG C.
Further, the time of described cracking is 3 seconds.
Further, the parameter of described gas chromatography is: Stationary liquid is polyglycol, and carrier gas is helium, constant current mode, flow velocity is 1.5mL/min, and injector temperature is 250 DEG C, split ratio is 100:1, column temperature takes temperature-programmed mode: initial temperature 50 DEG C, keeps 2min, is then warming up to 200 DEG C with 3 DEG C/min, keep 1min, finally be warming up to 260 DEG C with 2 DEG C/min, keep 5min, equilibration time is 1min.
Further, described mass spectrographic parameter is: transmission line temperature 280 DEG C, and ionization mode is electron bombardment ionization source, monitoring mode is that full scan pattern is qualitative, area normalization standard measure, sweep limit 29-550amu, ionizing energy 70eV, ion source temperature 280 DEG C, solvent delay is 4.5min.
Further, described cracking adopts cracking instrument, and the parameter of cracking is: initial temperature 60 DEG C, keeps 2s, is warming up to required cracking temperature with 10 DEG C/s, keeps 3s; Cracking atmosphere is air, and gas flow is 276mL/min; Cracking instrument interface standby temperature: 50 DEG C, working temperature 200 DEG C; Cracking instrument clack box temperature 200 DEG C, cracking instrument transmission line temperature 200 DEG C.
The present invention, in experimentation, simulates the temperature setting of low temperature cigarette heating part by setting different cracking temperatures; Utilize pressurized air as cracking reaction gas to simulate air ambient during low temperature cigarette heating; To carry out under same laboratory sample same temperature 8-12 time, each pyrolysis time is the aspiration procedure that the low temperature pyrolyzer of 2-4 second (carrying out statistical estimation according to smoker's tobacco habit) simulates a low temperature cigarette.Analyze in pyrolysis gas injection gas chromatography-mass spectrometer after each cracking.
Low temperature cigarette is in the process of heating, no matter be the mode of heating or outer rim heating in the middle of adopting, being heated of cigarette shreds part is uneven, but all presents the trend progressively decayed.The present invention, based on Marlboro iQOS low temperature cigarette, measures the heating-up temperature of heating rod by temperature measuring set, have selected the flue gas release conditions of 150 DEG C, 195 DEG C and 246 DEG C three temperature spots to simulate the flue gas release conditions of the flue gas of whole cigarette.
Finally, obtain the data of 8-12 (preferably 10 times) cracking under low temperature cigarette same temperature by experiment, these data are carried out mass spectrogram parsing and statistical study, the constituent title of each low temperature cigarette flue gas and the percentage contents of each material can be obtained.Meanwhile, by the content of more every secondary data, the Changing Pattern of low temperature cigarette smoke components in aspiration procedure can be simulated.
The present invention utilizes ripe pyrolysis technology to simulate the heating process of low temperature cigarette, in conjunction with gas chromatography-mass spectrometry instrument analytical approach, low temperature cigarette smoke components is analyzed, draw the material composition of low temperature cigarette flue gas and the percentage contents of each material, the flue gas content of suction low temperature cigarette process can be drawn simultaneously, provide important references to low temperature cigarette flue gas analysis and product development.
Accompanying drawing explanation
Fig. 1 represents instrument connection diagram.
Fig. 2 represents the total ion current figure of flue gas at Marlboro low temperature cigarette 195 DEG C.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The present embodiment provides a kind of low temperature cigarette fume component analysis method, and this embodiment is for the Marlboro iQOS low temperature cigarette sample of Fei Mo company, and select heating-up temperature point to be 195 DEG C, instrument connection diagram is as Fig. 1.
1, instrument: gas chromatograph-mass spectrometer (GCMS) (GC-MS) instrument flies you ISQ of generation mono-level Four bar gas chromatograph-mass spectrometer for match is silent, thermal cracking instrument is CDS5200 type cracking instrument.
2, sample filling: get a low temperature cigarette, take out tobacco section, get and put in the middle of cracking tube in right amount, cracking tube two end plug silica wool, weigh in the balance and get weight, generally take weight at about 0.01g, sample is to be measured.
3, instrument parameter
Gas chromatograph parameters is: analytical column is DB-WAXETR quartz capillary column (60m × 0.25mmid0.25 μm of film, the highest tolerable temperature 280 DEG C) (Stationary liquid is polyglycol), carrier gas is helium, purity >=99.999%, constant current mode, flow velocity is 1.5mL/min, injector temperature is 250 DEG C, split ratio is 100:1, and column temperature takes temperature-programmed mode: initial temperature 50 DEG C, keeps 2min, then 200 DEG C are warming up to 3 DEG C/min, keep 1min, be finally warming up to 260 DEG C with 2 DEG C/min, keep 5min.Equilibration time is 1min.
Mass spectrometry parameters is: transmission line temperature 280 DEG C, ionization mode: electron bombardment ionization source (EI), monitoring mode: full scan pattern is qualitative, area normalization standard measure, sweep limit 29-550amu, ionizing energy: 70eV, ion source temperature 280 DEG C, solvent delay: 4.5min.Standard diagram storehouse: NIST.
Thermal cracking parameter is: cracking heating schedule: initial temperature 60 DEG C, keeps 2s, rises to 195 DEG C with 10 DEG C/s, keeps 3s; Cracking atmosphere: air, gas flow is 276mL/min; Cracking instrument interface standby temperature: 50 DEG C, working temperature 200 DEG C; Cracking instrument clack box temperature: 200 DEG C, cracking instrument transmission line temperature: 200 DEG C.
4, data processing
1) the qualitative and semi-quantitative analysis of low temperature cigarette flue gas
Peak area gives integration higher than maximum peak (non-solvent peak) peak area 0.1%, and applying mass spectrum spectrum storehouse, to carry out retrieval qualitative, and peak area normalization percentage composition (percentage contents) carries out quantitatively.
In formula:
The peak area normalization percentage composition (%) of Xi---something;
The peak area of Mi---something;
Σ mi---material total mark area;
With the mean value of twice replicate determination for measurement result, the relative deviation of twice replicate determination maximum peak peak area normalization percentage composition is not more than 10%.
2) expression of results
Test findings is as table 1, and attached Marlboro low temperature cigarette flue gas total ion current figure, see Fig. 2.
Flue gas Principle components analysis report at table 1 Marlboro low temperature cigarette 195 DEG C
2.1 Marlboro low temperature cigarette 10 times smoke components changes.
At 195 DEG C, 10 times are carried out to same Marlboro low temperature cigarette sample and repeats cracking, the percentage contents of principal ingredient in flue gas is carried out statistical study, as shown in table 2.
10 the smoke components changes of table 2 Marlboro low temperature cigarette
Claims (9)
1. a low temperature cigarette fume component analysis method, is characterized in that, gets low temperature cigarette pipe tobacco or thin slice, and under air ambient, cracking is carried out in heating, and the temperature of described cracking is 145-250 DEG C, and the time of cracking is 2-4 second; Flue gas after cracking is input to gas chromatograph-mass spectrometer (GCMS) and carries out constituent analysis, then carry out test data processing the percentage contents that can obtain each material in flue gas.
2. analytical approach as claimed in claim 1, it is characterized in that, described cracking is carried out 8-12 time under same cracking temperature, and the time of each cracking is 2-4 second, the flue gas after each cracking is input to gas chromatograph-mass spectrometer (GCMS) and carries out constituent analysis.
3. analytical approach as claimed in claim 1, is characterized in that, described cracking temperature is selected from following temperature range 145-155 DEG C, 190-200 DEG C and 240-250 DEG C.
4. the analytical approach as described in any one of claim 1-3, is characterized in that, selects multiple cracking temperature to carry out cracking respectively.
5. analytical approach as claimed in claim 4, is characterized in that, described cracking temperature selects following three temperature spots: 150 DEG C, 195 DEG C and 246 DEG C.
6. the analytical approach as described in claim 1-3, is characterized in that, the time of described cracking is 3 seconds.
7. analytical approach as claimed in claim 1, it is characterized in that, the parameter of described gas chromatography is: Stationary liquid is polyglycol, carrier gas is helium, constant current mode, and flow velocity is 1.5mL/min, injector temperature is 250 DEG C, and split ratio is 100:1, and column temperature takes temperature-programmed mode: initial temperature 50 DEG C, keep 2min, then be warming up to 200 DEG C with 3 DEG C/min, keep 1min, be finally warming up to 260 DEG C with 2 DEG C/min, keep 5min, equilibration time is 1min.
8. analytical approach as claimed in claim 1, it is characterized in that, described mass spectrographic parameter is: transmission line temperature 280 DEG C, ionization mode is electron bombardment ionization source, and monitoring mode is that full scan pattern is qualitative, area normalization standard measure, sweep limit 29-550amu, ionizing energy 70eV, ion source temperature 280 DEG C, solvent delay is 4.5min.
9. analytical approach as claimed in claim 1, is characterized in that, described cracking adopts cracking instrument, and the parameter of cracking is: initial temperature 60 DEG C, keeps 2s, is warming up to required cracking temperature with 10 DEG C/s, keeps 3s; Cracking atmosphere is air, and gas flow is 276mL/min; Cracking instrument interface standby temperature: 50 DEG C, working temperature 200 DEG C; Cracking instrument clack box temperature 200 DEG C, cracking instrument transmission line temperature 200 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
| CN108593487B (en) * | 2018-04-02 | 2020-09-15 | 云南中烟工业有限责任公司 | Thermogravimetric analysis method for identifying safe temperature window of low-temperature cigarette |
| CN112129726A (en) * | 2020-09-23 | 2020-12-25 | 上海烟草集团有限责任公司 | Method, system, medium and equipment for evaluating uniformity of cut stems of cigarettes |
| CN112899081A (en) * | 2021-01-19 | 2021-06-04 | 云南中烟工业有限责任公司 | Preparation method and application of DGP (DGP-protein) substance |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG65649B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the assessment of the colour and the colour classification of tobaccos |
| CN103698431A (en) * | 2013-12-27 | 2014-04-02 | 云南烟草科学研究院 | Method for measuring glycerinum and 1,2-propylene glycol in cigarettes, electronic cigarettes and low-temperature cigarettes |
-
2015
- 2015-11-17 CN CN201510788851.1A patent/CN105467025B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG65649B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the assessment of the colour and the colour classification of tobaccos |
| CN103698431A (en) * | 2013-12-27 | 2014-04-02 | 云南烟草科学研究院 | Method for measuring glycerinum and 1,2-propylene glycol in cigarettes, electronic cigarettes and low-temperature cigarettes |
Non-Patent Citations (4)
| Title |
|---|
| 孔浩辉等: "裂解气相色谱-质谱联用法分析卷烟燃吸产物", 《理化检验-化学分册》 * |
| 曾金等: "裂解－气相色谱－质谱法测定卷烟燃吸产物的色谱柱选择", 《理化检验-化学分册》 * |
| 董宁宁: "不同温度条件下卷烟的热裂解GC/MS研究", 《质谱学报》 * |
| 赵国玲等: "热裂解气质联用技术研究烟草成分对烟气组分的影响", 《应用化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593487B (en) * | 2018-04-02 | 2020-09-15 | 云南中烟工业有限责任公司 | Thermogravimetric analysis method for identifying safe temperature window of low-temperature cigarette |
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
| CN108776184B (en) * | 2018-06-13 | 2020-10-13 | 湖北中烟工业有限责任公司 | Method for detecting smoke components of heated non-combustible cigarette |
| CN112129726A (en) * | 2020-09-23 | 2020-12-25 | 上海烟草集团有限责任公司 | Method, system, medium and equipment for evaluating uniformity of cut stems of cigarettes |
| CN112899081A (en) * | 2021-01-19 | 2021-06-04 | 云南中烟工业有限责任公司 | Preparation method and application of DGP (DGP-protein) substance |
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