CN101241055B - Tobacco pyrolytic cracking analytical method - Google Patents
Tobacco pyrolytic cracking analytical method Download PDFInfo
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- CN101241055B CN101241055B CN2008100263745A CN200810026374A CN101241055B CN 101241055 B CN101241055 B CN 101241055B CN 2008100263745 A CN2008100263745 A CN 2008100263745A CN 200810026374 A CN200810026374 A CN 200810026374A CN 101241055 B CN101241055 B CN 101241055B
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Abstract
Disclosed is an analysis method for tobacco thermal cracking, simulating the burning state during the cigarette smoking with different temperature areas set for low-temperature thermal purging of samples before a high-temperature cracking, and then products being introduced into a test equipment for qualitative and quantitative analysis. The invention realizes a complete simulation of the cigarette smoking process by the thermal cracking equipment, more close to the substance release state in the cigarette smoking process, facilitating a follow-up accurate detection and analysis of the tobacco and the combustion product thereof.
Description
Technical field
The invention belongs to technical field of analysis and detection, be specifically related to one and grow tobacco and the analytical approach of produce pyrolytic cracking dispensing product.
Background technology
The chemical constitution of cigarette shreds and cigarette smoke exist necessarily gets in touch, smoke components be pipe tobacco by burn, complicated processes such as cracking, degraded, distillation form, wherein cracking is a considerable link.
The cracking process of cigarette is very complicated, is difficult to its temperature of combustion, burning situation are controlled, and researchs and analyses difficulty.For this reason, there is the scholar to adopt the thermal cracking instrument that tobacco sample is carried out cracking, can realizes process simulation cigarette burning.Adopt this mode can control the condition of cigarette thermal cracking easily, for example temperature, environment etc., and because cracker can directly be connected with analytical equipment, do not need through stages such as flue gas trapping, extractions, not only simplify analysis operation greatly, and helped the analysis of trace in the flue gas or trace components.Therefore, this analytical technology has obtained application gradually in the tobacco research field.
In the prior art, the process that adopts apparatus for thermal cleavage to measure tobacco and produce pyrolytic cracking dispensing product thereof is: the thermal cracking that realizes sample by the apparatus for thermal cleavage TRANSIENT HIGH TEMPERATURE; Thermal cracking products has been discharged in the closed container, captures thermal cracking products by solid-phase extraction device, or brings thermal cracking products into the absorption hydrazine by carrier gas is mobile; The material that is captured in solid-phase extraction device or the absorption hydrazine is imported gas chromatograph-mass spectrometer (GCMS), carry out qualitative and detection by quantitative.The test method that also has is, after adopting apparatus for thermal cleavage high temperature to realize the sample thermal cracking, flows by carrier gas and directly to bring pyrolysis product into detecting instrument and carry out analyzing and testing.
The problem and shortage that existing method exists: by TRANSIENT HIGH TEMPERATURE cracking tobacco sample, ignored in the cigarette smoking process, not only have burning and Pintsch process, also there are chemical reactions such as distillation, destructive distillation in Pintsch process mainly at cigarette burning awl and near zone thereof.Cigarette burning awl temperature is usually at 700～1200 ℃, temperature around the cracking zone is at 400～700 ℃, distillation zone temperature near aspiration end generally is lower than 400 ℃, temperature behind the burning line sharply descends, thereafter dropped to 200 ℃ less than 2mm place temperature, the temperature of flue gas has had only 30～50 ℃ when entering the oral cavity.And also can see from existed test results, for the characteristic feature thing nicotine in the cigarette smoke, detected value under existing TRANSIENT HIGH TEMPERATURE cracking condition, doubly increase then with thermal cracking temperature rising XianCheng and slightly to descend or raise and reduce rapidly with temperature, " when temperature reaches 800 ℃, almost completely cleaved ".This with known, cigarette smoke in the nicotine burst size contradicted by the less conclusion of cigarette burning temperature effect.That is to say that simulate cigarette burning in existing thermal cracking mode, there is notable difference in both material release conditions.
Summary of the invention
The purpose of this invention is to provide a kind of new tobacco pyrolytic cracking analytical method.
The objective of the invention is to realize by following technical solution:
A kind of tobacco pyrolytic cracking analytical method is provided, may further comprise the steps:
(1) after tobacco sample is put into thermal cracker, carry out the first step and purge, gaseous purge stream imports the absorption hydrazine;
(2) intensification and second step purge, and gaseous purge stream imports adsorbs hydrazine;
(3) sample thermal cracking, thermal cracking products import the absorption hydrazine;
(4) capture (1), (2) and (3) gaseous purge stream and thermal cracking products and carry out analyzing and testing.
It is 30～100 ℃ that the described first step of step (1) purges temperature, and the gaseous purge stream flow velocity is 20～60mL/min, and the time that hot blow is swept is 5s～5min.
The described intensification of step (2) is that the programming rate with 0.05～1 ℃/ms is warming up to 200 ℃.
Intensification and purge time that described second step purges are 0～20s.
The described thermal cracking of step (3) is warming up to 400～1200 ℃ with the programming rate of 5～20 ℃/ms.
The described thermal cracking time cycle is 10～30s, comprises the required time of heating up.
The present invention simulates the fired state of cigarette aspiration procedure, and different temperature provinces is set, and at first carries out the low temperature hot blow and sweep before sample is carried out Pintsch process, then product is imported checkout equipment together, carries out qualitative, quantitative test.
The invention has the beneficial effects as follows: realized with the complete simulation of apparatus for thermal cleavage,, helped cigarette and goods products of combustion thereof are carried out follow-up accurate detection and analysis more near cigarette smoking process material release conditions to the cigarette smoking process.
Embodiment
Embodiment 1
1, key instrument and material
The GC6890N/5975B gas chromatography instrument of U.S. Agilent company; 5200 thermal cracking instrument of CDS company.
Tobacco sample: domestic certain famous cigarette product, pulverize the back and cross 80 mesh sieves.
2, method
Experimental procedure is as follows:
(1) after sample is put into the thermal cracking instrument, it is 30～100 ℃ that temperature is set, with the combination gas of the inert gas (nitrogen or helium) of 20%～100% oxygen and 80%～0% as gaseous purge stream, by the original carrier gas passage of thermal cracking instrument tobacco sample being carried out the first step purges, the gaseous purge stream flow velocity is 20～60mL/min, the time that hot blow is swept is 5s～5min, and gaseous purge stream imports the absorption hydrazine;
(2) programming rate with 0.05～1 ℃/ms is warming up to 200 ℃, carries out the second step purging, and intensification is 0～20s with purge time, and gaseous purge stream imports the absorption hydrazine;
(3) programming rate with 5～20 ℃/ms is warming up to 400～1200 ℃, and sample carries out thermal cracking, and thermal cracking products imports the absorption hydrazine.The thermal cracking time cycle is 10～30s, comprises the required time of heating up.
(5) capture step (1), (2) and (3) gaseous purge stream and thermal cracking products and carry out analyzing and testing.
Testing result to thermal cracking releasing product nicotine is: 2mg flue-cured tobacco offal A, nicotine burst size when final thermal cracking temperature is 400 ℃ is 7.736ug, is 8.571ug in the time of 600 ℃, is 8.423ug in the time of 800 ℃, being 8.215ug in the time of 1000 ℃, is 8.079ug in the time of 120 ℃.According to laboratory test results, the nicotine burst size under the highest different thermal cracking temperature is close substantially, and relative standard deviation is less than 4%, and is similar to the cigarette smoking situation of reality.
Claims (1)
1. tobacco pyrolytic cracking analytical method is characterized in that may further comprise the steps:
(1) after tobacco sample is put into thermal cracker, carry out the first step and purge, gaseous purge stream imports the absorption hydrazine, and it is 30～100 ℃ that the described first step purges temperature, and the gaseous purge stream flow velocity is 20～60mL/min, and the time that hot blow is swept is 5s～5min;
(2) heat up and carried out for second step and purge, gaseous purge stream imports the absorption hydrazine, and described intensification is warming up to 200 ℃ with the programming rate of 0.05～1 ℃/ms, and intensification and purge time that described second step purges are 0～20s;
(3) sample is warming up to 400～1200 ℃ with the programming rate of 5～20 ℃/ms and carries out thermal cracking, and thermal cracking products imports the absorption hydrazine; The described thermal cracking time cycle is 10～30s, comprises the heating-up time;
(4) capture step (1), (2) and (3) gaseous purge stream and thermal cracking products and carry out analyzing and testing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100263745A CN101241055B (en) | 2008-02-20 | 2008-02-20 | Tobacco pyrolytic cracking analytical method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100263745A CN101241055B (en) | 2008-02-20 | 2008-02-20 | Tobacco pyrolytic cracking analytical method |
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| CN101241055A CN101241055A (en) | 2008-08-13 |
| CN101241055B true CN101241055B (en) | 2011-04-06 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692076B (en) * | 2009-10-19 | 2012-01-04 | 中国烟草总公司郑州烟草研究院 | Infrared oven and GC-MS based method and infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes |
| CN101806685B (en) * | 2010-04-22 | 2011-11-23 | 上海烟草集团有限责任公司 | Tobacco aerobic cracking analysis system |
| CN101871922B (en) * | 2010-06-18 | 2012-07-04 | 云南烟草科学研究院 | Method for pyrolyzing tobacco additive and trapping and analyzing pyrolysis product |
| CN102735775A (en) * | 2011-04-06 | 2012-10-17 | 云南烟草科学研究院 | On-line entrapment and sample introduction method for gas chromatography-mass spectrometry analysis of pyrolyzate of material used for cigarette |
| CN102520095A (en) * | 2011-12-30 | 2012-06-27 | 广东中烟工业有限责任公司 | Method for detecting tobacco benzene material generating quantity by using thermal cracking |
| CN104266872B (en) * | 2014-09-19 | 2017-01-25 | 国家烟草质量监督检验中心 | Turntable type smoking machine collecting device with adsorption tube and analytical test method of collecting device |
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