CN108593487B - Thermogravimetric analysis method for identifying safe temperature window of low-temperature cigarette - Google Patents
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Abstract
The invention discloses a thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette, which comprises the steps of heating and pyrolyzing the low-temperature cigarette in a thermogravimetric analyzer to obtain thermal analysis curve information and escaping component information of the low-temperature cigarette, and integrating the two aspects of information to identify the safe temperature window of the low-temperature cigarette. According to the method, a thermochemical reaction model is established by presuming the pyrolysis reaction mechanism and the target smoke component generation mechanism of the low-temperature cigarette, and the method for promoting the generation of the beneficial components and inhibiting the generation of harmful substances is researched, so that the pyrolysis reaction of the low-temperature cigarette is orderly carried out in a controllable state according to an ideal direction.
Description
Technical Field
The invention belongs to the technical field of chemical test analysis, and particularly relates to a thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette.
Technical Field
The thermal analysis technique is a very important analysis and test method for studying various transformations and reactions of materials under the control of temperature program, such as dehydration, crystallization, melting, evaporation, phase transition, and the thermal decomposition process and reaction kinetics of various inorganic and organic materials. As one of the conventional thermal analysis techniques, the thermogravimetric/differential thermal analysis is a thermal analysis technique for measuring the relationship between the mass of a substance, the mass increase due to thermal change, the mass loss or the heat absorption, the heat release and the temperature by using a thermobalance at a program control temperature, has the advantages of simple and convenient instrument operation, high accuracy, sensitivity, rapidness, sample quantification and the like, and is widely applied to the fields of inorganic, organic, chemical, metallurgy, medicine, food, tobacco, energy, biology and the like.
The single-drop microextraction technology is a novel and environment-friendly sample pretreatment technology, integrates extraction and enrichment, and has the characteristics of low cost, simple device, easiness in operation, small organic solvent consumption, high enrichment efficiency and the like. Single-drop microextraction is performed by suspending a drop of extraction solvent from the tip of a conventional GC micro-syringe needle, then either by dipping in the sample solution or suspending in the sample headspace, allowing the analyte to transfer from the aqueous phase to the organic phase (extraction solvent), and withdrawing the organic droplet back into the syringe over time and transferring to a GC or other analytical system for analysis.
The automatic continuous liquid drop micro-extraction device is a novel headspace-single drop micro-extraction technology for automatically and continuously supplementing liquid drops under the condition of flowing carrier gas, is simple and convenient to operate, high in extraction speed and high in automation degree, realizes automatic continuous supplement and automatic collection of liquid drops of extraction liquid, and provides technical support for the application of the single drop micro-extraction technology in the field of thermogravimetric escaping component qualitative and quantitative analysis.
The low-temperature cigarette is used as a novel tobacco product, the cigarette is heated by using a special heat source, the highest temperature is generally not more than 500 ℃, tar and harmful components generated by combustion are reduced, and compared with the traditional cigarette, the low-temperature cigarette has lower harmfulness, and the research of the low-temperature cigarette is widely concerned. The heating temperature of the low-temperature cigarette has an important influence on smoke components, and in order to prevent complex pyrolysis reaction and inhibit harmful smoke components, the heating temperature needs to be controlled within a safe temperature range, however, a recognition analysis method related to a safe temperature window of the low-temperature cigarette is rarely reported.
Disclosure of Invention
The invention provides a thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette.
The invention aims to simulate the heating process of a low-temperature cigarette by using the programmed temperature rise of a thermogravimetric analyzer under the condition of inert or synthetic air, and provides an effective and feasible analysis method for the identification and analysis of a low-temperature cigarette safety temperature window by observing the thermal analysis curve of the cigarette and the escape behavior information of smoke components.
The invention aims to obtain thermal analysis curves of low-temperature cigarettes by using a thermogravimetric analyzer and thermal analysis software, wherein the thermal analysis curves comprise a thermogravimetric curve, a differential thermal curve, a time-temperature curve and a sample temperature-reference temperature curve.
The invention aims to perform thermogravimetric escape component analysis by using an automatic liquid drop continuous micro-extraction device and a combined detection instrument, realize qualitative and relative quantitative analysis on low-temperature cigarette smoke components and obtain the change rule of the low-temperature cigarette smoke components.
The invention aims to monitor the escape behavior of low-temperature cigarette smoke components in the heating process, comb and analyze the complex thermochemical reaction generated by low-temperature cigarette products by researching smoke components and change rules thereof, and realize the reverse analysis and process reference of similar products by means of low-temperature cigarette component analysis.
The invention aims to presume the pyrolysis reaction mechanism and the target smoke component generation mechanism of the low-temperature cigarette, establish a thermochemical reaction model, study the method for promoting or inhibiting the generation of target products and realize the ordered implementation of the pyrolysis reaction of the low-temperature cigarette in a controllable state according to an ideal direction.
The invention discloses a thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette, which has the technical scheme as follows:
a thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette is characterized in that the low-temperature cigarette is subjected to heating pyrolysis in a thermogravimetric analyzer to obtain thermal analysis curve information and escaping component information of the low-temperature cigarette, and the safe temperature window of the low-temperature cigarette is identified by integrating the two aspects of information.
Preferably, it comprises the following steps:
putting the cut tobacco of the low-temperature cigarette into a thermogravimetric analyzer, connecting the cut tobacco with an automatic liquid drop continuous micro-extraction device, and balancing for 5-15 min in an inert or synthetic air atmosphere;
secondly, starting a thermogravimetric analyzer, setting the temperature rise rate to be 5-30 ℃/min and the temperature rise range to be 25-900 ℃, starting detection in an inert or synthetic air atmosphere, and recording a thermal analysis curve;
starting the automatic liquid drop continuous micro-extraction device to extract and enrich the thermogravimetric escaping smoke components, and collecting the extraction liquid drops to a sample injection bottle at intervals of fixed temperature intervals;
starting a combined detecting instrument for analysis, and acquiring the component information of the escaped smoke from the collected liquid drops;
fifthly, obtaining the information of the escaped smoke components according to the step IV, and drawing a peak area-temperature curve of the escaped smoke components to obtain an escaped behavior curve of the escaped smoke components of the low-temperature cigarette in the temperature rising process;
sixthly, selecting the concerned smoke components of the low-temperature cigarette product, comparing the thermal analysis curve in the step II with the escape behavior curve in the step V, finding out the main temperature interval generated by certain components, and obtaining the safety temperature window for identifying the low-temperature cigarette.
Preferably, the thermal analysis curve of step two includes: thermogravimetric curves, differential thermal curves and time-temperature curves.
Preferably, the combined detection instrument of the step (iv) includes: gas chromatography, liquid chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, and capillary electrophoresis analyzer
The invention has the beneficial effects that:
1. according to the method, the thermal analysis software records the thermal analysis curve of the low-temperature cigarette, and the automatic droplet continuous micro-extraction device synchronously performs on-line extraction and enrichment of smoke components at intervals of fixed temperature intervals, so that synchronous correspondence between thermal analysis information and smoke component information is realized, and sequential development of later data analysis is facilitated.
2. The method of the invention utilizes the automatic liquid drop continuous micro-extraction device to extract and enrich the series of smoke components in different temperature intervals into the series of liquid drops, has the advantages of on-line synchronization, simplicity, convenience and high efficiency, is convenient for the combined analysis with a plurality of subsequent detection instruments, and realizes the multi-angle and all-directional investigation of the smoke component information.
3. The method of the invention researches the smoke components and the change rule thereof by monitoring the escape behavior of the smoke components of the low-temperature cigarette in the heating process, can comb and analyze the complex thermochemical reaction generated by the low-temperature cigarette, and realizes the reverse analysis and process reference of similar products by means of the original component analysis of the low-temperature cigarette.
4. By analyzing and mining the information data, the method can conjecture the pyrolysis reaction mechanism and the target smoke component generation mechanism of the low-temperature cigarette, establish a thermochemical reaction model, research the method for promoting the generation of the beneficial components and inhibiting the generation of the harmful substances, and finally realize the ordered implementation of the pyrolysis reaction of the low-temperature cigarette in a controllable state according to the ideal direction.
Drawings
FIG. 1 is a Thermogravimetric (TG), Differential Thermogravimetric (DTG), differential thermal (DSC), sample temperature (Ts) -reference temperature (Temp) curve of a low temperature cigarette sample according to an embodiment of the present invention;
FIG. 2 is a total ion flow chromatogram of smoke components of a low-temperature cigarette sample in a series of temperature intervals according to an embodiment of the invention;
FIG. 3 is a graph showing the escape behavior of the main smoke components of a sample of a low temperature cigarette according to an embodiment of the present invention;
FIG. 4 is a graph showing the escaping behavior of some harmful smoke components from a sample of a low-temperature cigarette according to an embodiment of the present invention.
Detailed Description
In order to further illustrate the technical means and efficacy of the present invention, the application and embodiments of the thermogravimetric analysis method for identifying the safe temperature window of a low-temperature cigarette according to the present invention are described in detail below with reference to the accompanying drawings and examples, but the present invention is not limited thereto.
Example (b): and analyzing and identifying the safe temperature window of the low-temperature cigarette by using a thermal analyzer-droplet continuous micro-extraction-gas chromatography-mass spectrometry.
And intercepting the tobacco shred part at the front end of the low-temperature cigarette as an experimental sample. And starting a thermal analyzer, accurately weighing 200mg of sample in the thermogravimetric crucible, and then closing the furnace body. Setting the temperature programming conditions as follows: heating from 40 deg.C to 500 deg.C at a heating rate of 10 deg.C/min, and maintaining for 10 min. The carrier gas is dry air, and the flow rate is 200 mL/min. Connecting a thermal analyzer with an automatic droplet continuous micro-extraction device, and balancing the system in a dry air atmosphere for 10 min.
Starting thermal analysis software to start thermogravimetric analysis, introducing dry air to detect, and recording a thermal analysis curve, such as a Thermogravimetric (TG), differential thermal (DSC) and sample temperature (Ts) -reference temperature (Temp) curve of a low-temperature cigarette sample shown in figure 1. And simultaneously starting the automatic droplet continuous micro-extraction device, using isopropanol as an internal standard substance to perform on-line extraction and enrichment of thermogravimetric escaping components, collecting the droplets of the extract into a sample injection bottle at intervals of 20 ℃, and rapidly and automatically replenishing new droplets by the device after each droplet taking.
According to the fluctuation of the DTG curve, as shown in FIG. 1, the temperature point T can be determined1、T2、T3、T4、T5The pyrolysis process of the sample before 500 ℃ is divided into 6 stages. Comparing the TG curve and the DTG curve, it can be seen that the weight loss of the sample starts at the initial stage of temperature rise before 100 ℃ and at T6The pre-weightlessness rate is continuously accelerated, and the post-weightlessness rate is continuously reduced until T1. Sample consisting of T1Heating to T2In the process at T7The maximum rate of weight loss for this phase is reached. At T2～T3And T4～T5In both phases, the DTG curve forms a downward spike (T)8、T9At) when the change in the rate of weight loss is most pronounced. T is3～T4The phase is sandwiched between the two rapid weight loss phases, and the sample slowly loses weight at a constant speed at the moment to form a platform phase of a DTG curve, and shows completely different weight loss characteristics from other phases. T is5The sample then enters a relatively flat weight loss process.
And (3) starting a gas chromatograph-mass spectrometer to analyze the collected series of liquid drops to obtain the escaped series of smoke component information, and referring to fig. 2, the total ion flow chromatogram of the smoke components of the low-temperature cigarette sample detected in a series of temperature intervals of 20 ℃. The gas chromatography detection conditions include: a chromatographic column: VOCOL capillary chromatography column (60m × 0.32mm × 1.8 μm); sample inlet temperature: 220 ℃; carrier gas: he (purity 99.999%); carrier gas flow: 1.2mL/min, column box temperature program: keeping at 40 deg.C for 4min, heating to 210 deg.C at a heating rate of 10 deg.C/min, and keeping for 10 min; split-flow sample injection is carried out, and the split-flow ratio is 1: 30. The mass spectrum detection conditions comprise: electron impact ion source (EI); electron energy: 70 eV; scanning range: m/z is 35-300; transmission line temperature: 220 ℃; ion source temperature: 220 ℃; the Nist 2005 and Wiley7 mass libraries were used for compound retrieval and qualitative analysis.
The temperature intervals selected in fig. 2 have certain representativeness in 6 pyrolysis stages, wherein 4 temperature intervals respectively include the temperature point T at the position where the sample undergoes rapid weight loss in the corresponding stage6～T9. The compound at retention time 5.0min in fig. 3 is isopropanol as an internal standard used in droplet microextraction, and the peak intensities of the internal standard are very close in each temperature interval. The other compounds are smoke components of the low-temperature cigarette sample, and the smoke component components in each stage are greatly different.
The series of smoke component information corresponds to the series of temperature intervals during the liquid drop collection one by one, peak area data of each smoke component and an internal standard substance in the series of temperature intervals in the chromatogram are extracted, and a peak area ratio-temperature curve of each smoke component/internal standard substance is drawn, namely an escape behavior curve of a pyrolysis product (smoke component) of the low-temperature cigarette in the temperature programming process. The method comprises the steps of screening out concerned components from a plurality of smoke components, comparing a thermal analysis curve with a pyrolysis product escape behavior curve, finding out a main temperature interval generated by the concerned components, comprehensively weighing harmful components and favorable components, finding out a temperature interval with more escaping favorable smoke components and less harmful components, and identifying a safe temperature window of the low-temperature cigarette product.
FIG. 3 is a curve of the escape behavior of the main smoke components of the low temperature cigarette sample. It can be seen that menthol is detected to escape at the initial stage of sample temperature rise, the escape amount reaches the peak value in the temperature range of 180-200 ℃, and the menthol almost completely escapes before 300 ℃. The experiment researches that the menthol taste sample has a lower temperature range for releasing menthol, so that the menthol taste can be more easily embodied by the product. Compared with the prior art, the temperature requirement of nicotine escape in the sample is high, the main escape temperature range is 160-280 ℃, and the nicotine still escapes after the main escape temperature range, but the relative escape amount is kept at a low level. Comparing the escape behavior curves of the two shows that the integral area of the menthol curve is obviously larger than that of the nicotine curve, which indicates that the relative escape amount of menthol is obviously higher than that of nicotine. From the integral area of the corresponding curve, the relative escape amount of acetic acid is second to menthol and nicotine, and the main escape interval is 180-360 ℃; the relative escape amount of the hydroxyacetone, the furfuryl alcohol, the glycerol and the glycerol monoacetate is much lower than that of the menthol and the nicotine, and the main escape interval is 200-320 ℃. By integrating the escape behavior information of each main smoke component, the lowest heating temperature of the low-temperature cigarette needs to be controlled to be more than 260 ℃ so that each main smoke component can better escape.
FIG. 4 is a curve of the escape behavior of all 14 benzene series in the smoke components of the low-temperature cigarette. The benzene series is a relatively concerned substance, and experiments show that a plurality of benzene series are found in smoke components. It can be seen that the relative emission of phenol is significantly higher than that of other benzene series, and the emission peak appears in the temperature range of 280-300 ℃, and the emission peak of acetic acid and hydroxyacetone also appears in the temperature range in fig. 3, which corresponds to the position of the first peak of the DTG curve in fig. 1. Compared with other benzene series curves, the method has the advantages that phenol escapes greatly before 380 ℃, and accounts for 80.38% of the total escape amount before 500 ℃; the benzyl alcohol escapes at the early stage of pyrolysis, and the main escape range is 120-280 ℃; the p-cresol and the phenol still have larger escape amount at 320-380 ℃, the temperature interval is just in a T3-T4 plateau period on a DTG curve, and the escape of most benzene series is obviously reduced or even stopped at the moment. The plateau stage blocks the escape of part of the benzene series into a front part and a rear part, and the escape of most of the benzene series is obviously increased or begins to escape after 380 ℃. The relative bleeding of the other benzene series, except phenol, before 380 ℃ was only 19.15% of the total bleeding before 500 ℃. From the information of the benzene series escaping behavior, the maximum heating temperature of the low-temperature cigarette needs to be controlled below 380 ℃, and the benzene series content of smoke except phenol can be greatly reduced compared with the higher temperature.
In conclusion, according to the escape behavior information of 9 main smoke components and all 14 benzene series, the safe temperature window of the low-temperature cigarette is 260-380 ℃.
Claims (3)
1. A thermogravimetric analysis method for identifying a safe temperature window of a low-temperature cigarette is characterized in that the method comprises the steps of heating and pyrolyzing the low-temperature cigarette in a thermogravimetric analyzer to obtain thermal analysis curve information and escaped smoke component information of the low-temperature cigarette, and integrating the two information so as to identify the safe temperature window of the low-temperature cigarette; the method comprises the following specific steps:
putting cut tobacco of a low-temperature cigarette into a thermogravimetric analyzer, connecting an automatic liquid drop continuous micro-extraction device, and balancing for 5-15 min;
secondly, starting a thermogravimetric analyzer, setting the temperature rise rate to be 5-30 ℃/min and the temperature rise range to be 25-900 ℃, and recording a thermal analysis curve;
starting the automatic liquid drop continuous micro-extraction device to extract and enrich the thermogravimetric escaping smoke components, and collecting the extraction liquid drops to a sample injection bottle at intervals of fixed temperature intervals;
starting the analysis step of the combined detecting instrument and the collected extraction liquid drops to obtain the information of the escaped smoke components;
fifthly, obtaining the information of the escaped smoke components according to the step IV, and drawing a peak area-temperature curve of the escaped smoke components to obtain an escaped behavior curve of the escaped smoke components of the low-temperature cigarette in the temperature rising process;
sixthly, selecting the concerned smoke components of the low-temperature cigarette product, comparing the thermal analysis curve in the step II with the escape behavior curve of the escaped smoke components in the step V, and finding out the main temperature interval generated by the concerned smoke components to obtain the safety temperature window for identifying the low-temperature cigarette.
2. The analytical method of claim 1, wherein the thermal analysis curve of step (ii) comprises: thermogravimetric curves, differential thermal curves and time-temperature curves.
3. The analytical method according to claim 1, wherein the combined measuring instrument of step (iv) comprises: a gas chromatography instrument, a liquid chromatography instrument, a gas chromatography-mass spectrometry instrument, a liquid chromatography-mass spectrometry instrument, and a capillary electrophoresis analysis instrument.
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| CN113049631B (en) * | 2021-03-24 | 2022-10-04 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction method for quantitative analysis of thermogravimetric escaping substances |
| CN114324452B (en) * | 2022-01-12 | 2024-07-02 | 中国科学院工程热物理研究所 | Detection and analysis method applied to critical characteristics in solid-liquid phase reaction process |
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