CN101241056B - Tobacco and its product pyrolytic cracking analytical method - Google Patents
Tobacco and its product pyrolytic cracking analytical method Download PDFInfo
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- CN101241056B CN101241056B CN200810026382XA CN200810026382A CN101241056B CN 101241056 B CN101241056 B CN 101241056B CN 200810026382X A CN200810026382X A CN 200810026382XA CN 200810026382 A CN200810026382 A CN 200810026382A CN 101241056 B CN101241056 B CN 101241056B
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Abstract
The invention discloses a tobacco and a thermal cracking analysis method of the product thereof. The tobacco sample undergoes high-temperature cracking under the condition of auxiliary gas. The product of thermal cracking is carried by the auxiliary gas into absorption hydrazine and trapped, heated for de-absorption, and guided into a detection device by carrier gas. The auxiliary gas is mixture of oxygen and inert gas. The invention realizes simulation of tobacco absorption by thermal cracking device, enables the thermal cracking product to be more close to releasing situation of tobacco absorption process by limiting component and flow speed of auxiliary gas precisely. The invention is beneficial for successive precise detection and analysis to tobacco and combustion product of product thereof.
Description
Technical field
The invention belongs to technical field of analysis and detection, be specifically related to measure the analytical approach of tobacco and produce pyrolytic cracking dispensing product thereof.
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 thermal cracking behavior of research cigarette and product thereof are significant for objectionable constituent in raising cigarette composition level, flavoring and casing level and the reduction flue gas.
But the burning 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, the analysis operation of simplifying greatly not only, and help 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: adopt thermal cracker, under certain flow rate of carrier gas, adopt TRANSIENT HIGH TEMPERATURE to realize the thermal cracking of sample, and thermal cracking products is directly imported analytical instrument by carrier gas, carrier gas is an inert gas, is generally nitrogen or helium; Or under atmospheric environment, in the airtight container, carry out the high temperature pyrolysis of sample, and then adopt solid-phase extraction device to carry out the extraction of cracking releasing product, analyze; Or adopt the mode of auxiliary gas, and oxygen concentration has only 5% in the auxiliary gas, carries out the Pintsch process of sample under 7mL/min secondary air speed, and the cracking releaser is adsorbed hydrazine absorption earlier, then again by desorption and carry out constituent analysis.
The problem and shortage that existing method exists: under inert gas environment, carry out the Pintsch process of tobacco sample, with cigarette smoking be that the situation of carrying out under atmospheric environment is not inconsistent fully, therefore can not effectively simulate the process that burns and sucks of cigarette; Carrying out the thermal cracking of sample under airtight atmospheric environment, ignored cigarette burning no matter be in aspiration procedure or smoldering process, all is to carry out under certain gas velocity, therefore also has very big defective; And adopting certain secondary air speed, oxygen concentration is low excessively, belongs to carry out the tobacco sample Pintsch process under anaerobic environment, and is also variant with the Actual combustion situation of cigarette.The analyzing and testing result of thermal cracking products can not reflect the process that the burns and sucks dispensing product situation of cigarette truly in the said method.
In the cigarette smoking process, according to the examination criteria of ISO, the gas velocity of its mouth end has reached 17.5mL/s (being 1.05L/min), and the cigarette degree of depth puffing regimens in Canada's health and the hygienic standard more requires gas velocity to reach 27.5mL/min; And in the smoldering process, the gas velocity of environment also requires to reach 200mm/s.Even as cigarette Zhi Caiyong punching dilution technology or when adopting high ventilative cigarette paper, the gas velocity of stub end is suction low; And the gas velocity when cigarette glows, much lower in the time of aspirating, but generally speaking, the gas velocity in the cigarette burning process is very high, cigarette burning is actually under oxygen-enriched environment and carries out.But in the different phase that cigarette burns and sucks, its gas velocity has than big-difference; Even and in aspiration procedure, the gas velocity of stub end distributes also also inhomogeneous, the air-flow of burning awl center is much lower than the outer rim of burning awl.Carry out the accurate analysis that cigarette and goods thereof burn and suck product, at first will seek the pyrolytic cracking analytical method that energy real simulation cigarette burns and sucks process.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of more real simulation cigarette and goods thereof to burn and suck the pyrolytic cracking analytical method of process.
By apparatus for thermal cleavage tobacco and goods thereof are carried out thermal cracking, the fired state of simulation cigarette aspiration procedure, mode is that the environment set with the tobacco sample thermal cracking is under certain gas velocity, oxygen-supplying amount reaches the thermal cracking environment more than 20%.
The objective of the invention is to realize by following technical solution:
Provide one to grow tobacco and produce pyrolytic cracking analytical method, tobacco sample carries out Pintsch process under the condition for auxiliary gas, thermal cracking products is gone into to adsorb hydrazine by the auxiliary band of gas and is captured, desorption by heating also imports detecting instrument by carrier gas, described auxiliary gas is the combination gas of oxygen and inert gas, and described oxygen content is 20～100% (percents by volume).
Described inert gas is nitrogen or helium.
The flow velocity of described auxiliary gas is 20mL/min～60mL/min.
The time of described thermal cracking is 10s～90s, comprises the required time of heating up.
Because the ability of absorption hydrazine is limit in the prior art, during cigarette burning the gas velocity of mouth end difficulty be adjusted to 1.05L/min (or 27.5mL/min), so the present invention adopts the oxygen content and the thermal cracking time of improving in the auxiliary gas to remedy above-mentioned defective, and has been determined by experiment oxygen content and the scope of thermal cracking time in the auxiliary gas.
The invention has the beneficial effects as follows: realized with the simulation of apparatus for thermal cleavage to the cigarette smoking process.Composition and flow velocity by the auxiliary gas of accurate definition make thermal cracking products more near cigarette smoking process material release conditions, help cigarette and goods products of combustion thereof are carried out follow-up accurate detection and analysis.
Embodiment
Further specify the present invention below in conjunction with specific 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
With the combination gas of oxygen and nitrogen or helium as auxiliary gas, secondary air speed is 20L/min～60mL/min, tobacco sample carries out Pintsch process under the condition for auxiliary gas, thermal cracking products is gone into to adsorb hydrazine by the auxiliary band of gas and is captured, desorption by heating also imports detecting instrument by carrier gas, carries out analyzing and testing.The time of described thermal cracking is 10s～90s, comprises the required time of heating up.
With said method 2mg flue-cured tobacco offal A is carried out thermal cracking, with the combination gas of oxygen and nitrogen as auxiliary gas, secondary air speed is got under the condition of 30mL/min, 800 ℃ of thermal cracking temperature, thermal cracking cycle 20s, the testing result that discharges product is separated in the GC/MS counterincision: during oxygen supply amount 20%, promptly with the situation of ambient atmosphere oxygen concentration 21% when close, value of detecting (with the clean peak height of abundance value representation) of releasing product accumulative total is 982.38 * 105Abs., and wherein accumulative total value of detecting of the fragrance matter that can identify is 453.68 * 105Abs..
Embodiment 2
Instrument and material are with embodiment 1.
With the combination gas of oxygen and nitrogen or helium as auxiliary gas, secondary air speed is 20L/min～60mL/min, tobacco sample carries out Pintsch process under the condition for auxiliary gas, thermal cracking products is gone into to adsorb hydrazine by the auxiliary band of gas and is captured, desorption by heating also imports detecting instrument by carrier gas, carries out analyzing and testing.The time of described thermal cracking is 10s～90s, comprises the required time of heating up.
With said method 2mg flue-cured tobacco offal A is carried out thermal cracking, with the combination gas of oxygen and helium as auxiliary gas, secondary air speed is got under the condition of 30mL/min, 800 ℃ of thermal cracking temperature, thermal cracking cycle 20s, the testing result that discharges product is separated in the GC/MS counterincision: under the situation under the oxygen-enriched environment, for example during oxygen supply amount 80%, value of detecting (with the clean peak height of abundance value representation) of releasing product accumulative total is 158.71 * 105Abs.; Wherein accumulative total value of detecting of the fragrance matter that can identify is 85.36 * 105Abs..
Claims (3)
1. one grow tobacco and produce pyrolytic cracking analytical method, tobacco sample carries out Pintsch process under the condition for auxiliary gas, thermal cracking products is gone into to adsorb hydrazine by the auxiliary band of gas and is captured, desorption by heating also imports detecting instrument by carrier gas, it is characterized in that described auxiliary gas is the combination gas of oxygen and inert gas, the shared volumn concentration of described oxygen is 20%～100%; The flow velocity of described auxiliary gas is 20mL/min～60mL/min.
2. according to described tobacco of claim 1 and produce pyrolytic cracking analytical method thereof, it is characterized in that described inert gas is nitrogen or helium.
3. according to described tobacco of claim 1 and produce pyrolytic cracking analytical method thereof, the time that it is characterized in that described Pintsch process is 10s～90s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810026382XA CN101241056B (en) | 2008-02-20 | 2008-02-20 | Tobacco and its product pyrolytic cracking analytical method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810026382XA CN101241056B (en) | 2008-02-20 | 2008-02-20 | Tobacco and its product pyrolytic cracking analytical method |
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| CN101241056A CN101241056A (en) | 2008-08-13 |
| CN101241056B true CN101241056B (en) | 2011-05-04 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102507846B (en) * | 2011-10-26 | 2013-12-11 | 河南中烟工业有限责任公司 | Method for measuring release quantity of ammonia in tobacco leaves |
| CN103884621B (en) * | 2014-03-18 | 2017-05-31 | 广东中烟工业有限责任公司 | A kind of device and method of inspection smoking material desorption rate |
| CN104266870B (en) * | 2014-09-19 | 2017-02-15 | 国家烟草质量监督检验中心 | Linear type smoking machine collecting device with adsorption tube and analytical test method of collecting device |
| 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 |
| CN104928026B (en) * | 2015-05-14 | 2018-10-23 | 安徽中烟工业有限责任公司 | A kind of fragrance and tobacco juice for electronic smoke promoting electronic cigarette organoleptic quality |
| CN112956732A (en) * | 2021-04-02 | 2021-06-15 | 河南中烟工业有限责任公司 | Tobacco lysate and preparation method thereof |
| CN112956731B (en) * | 2021-04-02 | 2022-09-23 | 河南中烟工业有限责任公司 | Method for preparing tobacco lysate by oxidative cracking of tobacco resources |
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