CN105467025B - A kind of low temperature cigarette fume component analysis method - Google Patents
A kind of low temperature cigarette fume component analysis method Download PDFInfo
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- CN105467025B CN105467025B CN201510788851.1A CN201510788851A CN105467025B CN 105467025 B CN105467025 B CN 105467025B CN 201510788851 A CN201510788851 A CN 201510788851A CN 105467025 B CN105467025 B CN 105467025B
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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
- 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
- G01N30/60—Construction of the column
- 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 kind of low temperature cigarette fume component analysis method, the analysis method is：Low temperature cigarette pipe tobacco or thin slice are taken, heats and is cracked under air ambient, the temperature of the cracking is 145 250 DEG C, the time of cracking is 24 seconds；Flue gas after cracking is input to gas chromatography-mass spectrometry and carries out constituent analysis, then the percentage contents of each material in flue gas can be obtained to test data progress processing.The present invention simulates the heating process of low temperature cigarette using ripe pyrolysis technology, with reference to gas chromatography-mass spectrometry device analysis method, low temperature cigarette smoke components are analyzed, draw the material composition of low temperature cigarette flue gas and the percentage contents of each material, the flue gas changes of contents of suction low temperature cigarette process can be drawn simultaneously, and important references are provided to low temperature cigarette flue gas analysis 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 a kind of incombustible cigarette of heating, and low temperature cigarette is heated (500 using special thermal source to pipe tobacco
Degree is following even lower), pipe tobacco is only heated without burning, pipe tobacco temperature far below traditional cigarette so that flue gas harmful chemicals into
Divide and bio-toxicity is greatly reduced, be closest to the tobacco product of cigarette, belong to tobacco product category.At present, low temperature cigarette is produced
Product are in development, although several tobacco companies have developed low temperature cigarette product, but product technology condition is also
It need to improve and perfect.
By investigating the low temperature cigarette product on overseas market, low temperature cigarette is with the hollow pen-like device of Cigarette size
Based on, heating part is separated with heated portion, heated portion is similar with common cigarette.For the cigarette of such low temperature cigarette
Qi leel analyses the document report there is not yet in this respect.By consulting the documents and materials related to low temperature cigarette, low temperature cigarette cigarette is had no
The patent and document of the detection of gas composition.
The content of the invention
Low temperature cigarette smoke components relative amount is detected present invention solves the technical problem that being to provide one kind and can analyze
Method, can be used for the exploitation for instructing tobacco company to low temperature cigarette.
The technical scheme is that there is provided a kind of low temperature cigarette fume component analysis method, take low temperature cigarette pipe tobacco or
Person's thin slice, heats under air ambient and is cracked, and the temperature of the cracking is 145-250 DEG C, and the time of cracking is 2-4 seconds；
Flue gas after cracking is input to gas chromatograph-mass spectrometer (GC-MS) and carries out constituent analysis, then test data progress is handled and can obtained
The percentage contents of each material in flue gas.
Further, the cracking is carried out 8-12 times under same cracking temperature, and the time of each cracking is 2-4 seconds,
Flue gas after each cracking is input to gas chromatograph-mass spectrometer (GC-MS) and carries out constituent analysis.
Further, the cracking temperature is selected from 145-155 DEG C, 190-200 DEG C and 240-250 DEG C of temperature below scope.
Further, multiple cracking temperatures are selected to be cracked respectively.
Further, the cracking temperature selection three below temperature spot：150 DEG C, 195 DEG C and 246 DEG C.
Further, the time of the cracking is 3 seconds.
Further, the parameter of the gas-chromatography is：Stationary phase is polyethylene glycol, and carrier gas is helium, constant current mode, stream
Speed is 1.5mL/min, and injector temperature is 250 DEG C, and split ratio is 100:1, column temperature takes temperature-programmed mode：50 DEG C of initial temperature,
2min is kept, then 200 DEG C are warming up to 3 DEG C/min, 1min is kept, finally 260 DEG C are warming up to 2 DEG C/min, 5min is kept,
Equilibration time is 1min.
Further, the mass spectrographic parameter is：280 DEG C of transmission line temperature, ionization mode is electron bombardment ionization source, monitoring side
Formula is that full scan pattern is qualitative, area normalization standard measure, scanning range 29-550amu, ionizing energy 70eV, ion source temperature
280 DEG C, solvent delay is 4.5min.
Further, the cracking is using cracking instrument, and the parameter of cracking is：60 DEG C of initial temperature, keeps 2s, with 10 DEG C/s
Required cracking temperature is warming up to, 3s is kept；Cracking atmosphere is air, and gas flow is 276mL/min；Crack instrument interface standby temperature
Degree：50 DEG C, 200 DEG C of operating temperature；Crack 200 DEG C of instrument clack box temperature, 200 DEG C of cracking instrument transmission line temperature.
The present invention is in experimentation, and by setting, different cracking temperatures simulates the temperature of low temperature cigarette heating part
Setting；Air ambient during low temperature cigarette heating is simulated by the use of compressed air as cracking reaction gas；To same laboratory sample
Progress 8-12 times, the low temperature that each pyrolysis time is 2-4 seconds (carrying out statistical estimation according to smoker's tobacco habit) under same temperature
Crack to simulate the aspiration procedure of a low temperature cigarette.Cracking gas is injected in gas chromatograph-mass spectrometer after cracking every time and carried out
Analysis.
Low temperature cigarette is during heating, whether by the way of centre heating or outer rim heating, cigarette shreds
It is partial it is heated be uneven, but all show the trend progressively decayed.The present invention is using Marlboro iQOS low temperature cigarettes as base
Plinth, the heating-up temperature of heating rod is measured by temperature measuring set, have selected 150 DEG C, 195 DEG C and 246 DEG C three temperature spots
Flue gas release conditions simulate the flue gas release conditions of the flue gas of whole branch cigarette.
Finally, the data that 8-12 times (preferably 10 times) are cracked are obtained under low temperature cigarette same temperature by experiment, by these
Data carry out mass spectrogram parsing and statistical analysis, can obtain the constituent title and each material of each low temperature cigarette flue gas
Percentage contents.Meanwhile, by the changes of contents of relatively more each data, low temperature cigarette can be simulated in aspiration procedure
The changing rule of smoke components.
The present invention simulates the heating process of low temperature cigarette using ripe pyrolysis technology, with reference to gas chromatography-mass spectrum
Instrument analytical method is combined, low temperature cigarette smoke components are analyzed, the material composition of low temperature cigarette flue gas is drawn and each
The percentage contents of material, while the flue gas changes of contents of suction low temperature cigarette process can be drawn, to low temperature cigarette flue gas
Analysis and product development provide important references.
Brief description of the drawings
Fig. 1 represents instrument connection diagram.
Fig. 2 represents the total ion current figure of flue gas at 195 DEG C of Marlboro low temperature cigarette.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The present embodiment provides a kind of low temperature cigarette fume component analysis method, and the embodiment is with the Marlboro of Fei Mo companies
Exemplified by iQOS low temperature cigarette samples, selection heating-up temperature point is 195 DEG C, instrument connection diagram such as Fig. 1.
1st, instrument：Gas chromatograph-mass spectrometer (GC-MS) (GC-MS) instrument is the silent winged generation that mono- level Four bar gas-chromatographies of ISQ of match
GC-MS, thermal cracking instrument is that CDS5200 types crack instrument.
2nd, sample is loaded：A low temperature cigarette is taken, tobacco section is taken out, takes and be put into right amount in the middle of cracking tube, cracking tube two
End plug silica wool, weighs in the balance and takes weight, typically weighs weight in 0.01g or so, sample is to be measured.
3rd, instrument parameter
Gas chromatograph parameters are：Analytical column is DB-WAXETR quartz capillary columns (0.25 μm of 60m × 0.25mm id
Film, 280 DEG C of highest tolerable temperature) (stationary phase is polyethylene glycol), carrier gas is helium, purity >=99.999%, constant current mode,
Flow velocity is 1.5mL/min, and injector temperature is 250 DEG C, and split ratio is 100:1, column temperature takes temperature-programmed mode：Initial temperature 50
DEG C, 2min is kept, then 200 DEG C are warming up to 3 DEG C/min, 1min is kept, 260 DEG C, holding are finally warming up to 2 DEG C/min
5min.Equilibration time is 1min.
Mass spectrometry parameters are：280 DEG C of transmission line temperature, ionizes mode：Electron bombardment ionization source (EI), monitoring mode：Full scan mould
Formula is qualitative, area normalization standard measure, scanning range 29-550amu, ionizing energy：70eV, 280 DEG C of ion source temperature, solvent
Delay：4.5min.Standard diagram storehouse：NIST.
Thermal cracking parameter is：Crack heating schedule：60 DEG C of initial temperature, keeps 2s, and 195 DEG C, holding are risen to 10 DEG C/s
3s；Crack atmosphere：Air, gas flow is 276mL/min；Crack instrument interface standby temperature：50 DEG C, 200 DEG C of operating temperature；Split
Solve instrument clack box temperature：200 DEG C, crack instrument transmission line temperature：200℃.
4th, data processing
1) low temperature cigarette flue gas is qualitative and semi-quantitative analysis
Peak area is integrated higher than maximum peak (non-solvent peak) peak area 0.1%, and application mass spectrum spectrum storehouse is examined
Rope is qualitative, and peak area normalization percentage composition (percentage contents) is quantified.
In formula：
The peak area normalization percentage composition (%) of Xi --- something；
The peak area of Mi --- something；
Σ mi --- material total mark area；
Using the average value of parallel determination twice as measurement result, the percentage of parallel determination maximum peak peak area normalization twice contains
The relative deviation of amount is not more than 10%.
2) result is stated
Result of the test such as table 1, and attached Marlboro low temperature cigarette flue gas total ion current figure, are shown in Fig. 2.
Flue gas Principle components analysis is reported at 195 DEG C of 1 Marlboro low temperature cigarette of table
2.1 smoke components of Marlboro low temperature cigarette 10 times change.
10 repetitions are carried out at 195 DEG C to same Marlboro low temperature cigarette sample to crack, by the phase of main component in flue gas
Statistical analysis is carried out to percentage composition, as shown in table 2.
2 Marlboro low temperature cigarette of table, 10 smoke components changes
Claims (3)
1. a kind of low temperature cigarette fume component analysis method, it is characterised in that take low temperature cigarette pipe tobacco or thin slice, in air ring
Heating is cracked under border, selects multiple cracking temperatures to be cracked respectively, and cracking temperature is selected from temperature below scope 145-155
DEG C, 190-200 DEG C and 240-250 DEG C, the cracking is carried out 8-12 times under same cracking temperature, and the time of each cracking is
2-4 seconds, the flue gas after each cracking is input to gas chromatograph-mass spectrometer (GC-MS) and carries out constituent analysis, then test data is entered
Row processing can obtain the percentage contents of each material in flue gas；
The parameter of the gas-chromatography is：Stationary phase is polyethylene glycol, and carrier gas is helium, and constant current mode, flow velocity is 1.5mL/
Min, injector temperature is 250 DEG C, and split ratio is 100:1, column temperature takes temperature-programmed mode：50 DEG C of initial temperature, keeps 2 min,
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
For 1min；
The mass spectrographic parameter is：280 DEG C of transmission line temperature, ionization mode is electron bombardment ionization source, and monitoring mode is full scan mould
Formula is qualitative, area normalization standard measure, scanning range 29-550amu, ionizing energy 70eV, 280 DEG C of ion source temperature, and solvent prolongs
It is 4.5min late；
The cracking uses cracking instrument, and the parameter of cracking is：60 DEG C of initial temperature, keeps 2s, needed for being warming up to 10 DEG C/s
Cracking temperature, keeps 3s；Cracking atmosphere is air, and gas flow is 276mL/min；Crack instrument interface standby temperature：50 DEG C, work
Make 200 DEG C of temperature；Crack 200 DEG C of instrument clack box temperature, 200 DEG C of cracking instrument transmission line temperature.
2. analysis method as claimed in claim 1, it is characterised in that the cracking temperature selects three below temperature spot：150
DEG C, 195 DEG C and 246 DEG C.
3. analysis method as claimed in claim 1, it is characterised in that the time of the cracking is 3 seconds.
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| CN201510788851.1A CN105467025B (en) | 2015-11-17 | 2015-11-17 | A kind of low temperature cigarette fume component analysis method |
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| 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 |
| 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 |
| CN112129726B (en) * | 2020-09-23 | 2023-04-25 | 上海烟草集团有限责任公司 | Method, system, medium and equipment for evaluating uniformity of tobacco stem shreds |
| 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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| CN103698431B (en) * | 2013-12-27 | 2015-09-09 | 云南烟草科学研究院 | The assay method of glycerine, 1,2-PD in a kind of cigarette, electronic cigarette and low temperature cigarette |
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