CN101995418B - Gathering device for thermoanalysis product - Google Patents
Gathering device for thermoanalysis product Download PDFInfo
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- CN101995418B CN101995418B CN2010102817362A CN201010281736A CN101995418B CN 101995418 B CN101995418 B CN 101995418B CN 2010102817362 A CN2010102817362 A CN 2010102817362A CN 201010281736 A CN201010281736 A CN 201010281736A CN 101995418 B CN101995418 B CN 101995418B
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Abstract
The invention discloses a gathering device for a thermoanalysis product, which is provided with a multi-port multi-angle blind nut, wherein a port is a gas inflowing port, a plurality of gas outflowing ports are distributed along the circumference of the multi-port multi-angle blind nut, the gas inflowing port of the multi-port multi-angle blind nut is communicated with the gas outlet end of a pyrolysis stove of a thermoanalysis meter, each gas outflowing port of the multi-port multi-angle blind nut is sequentially connected with a two-port valve and a Cambridge filter disc collector, and the gas inflowing port of the Cambridge filter disc collector is connected with the two-port valve, and the other outlet end of the Cambridge filter disc collector is connected with an on-line analysis mass spectrum, a gas collecting pocket or a solution trapping implement. By using the thermoanalysis meter to imitate the burning conditions of cigarette, the gathering device can be used for uninterruptedly and continuously gathering the tar state products and gas phase products at different temperatures in the burning and pyrolysis process of the tobacco, also can be used for repeatedly and effectively gathering the corresponding products in the same temperature section, and can realize the exact quantitative analysis on the thermoanalysis products.
Description
Technical field:
The present invention relates to a kind of gathering-device of tobacco components, a kind of gathering-device that is used for hot analytic process result of combustion of tobacco and pyrolysis product of more specifically saying so.
Background technology:
In the combustion process of cigarette, physics and chemistry route that tobacco is in complicacies such as process distillation under temperature and the continuous environmental baseline that changes of oxygen concentration, transfer, pyrolysis and burning can form several thousand kinds of products.Thermoanalysis technology is meant the physical property of measurement of species under program temperature control and one type of technology of temperature relation, and thermoanalysis technology method commonly used mainly comprises thermogravimetry (TG), differential thermal analysis (DTA) and DSC (DSC).The coupling technique of product analysis such as thermal analyzer and GC/MS instrument is the burning condition of simulation cigarette, and research result of combustion of tobacco process and product form the important tool of mechanism.
At present; Widely used heat is analyzed coupling technique in tobacco business; Generally be with direct couplings of product analysis instrument such as thermal analyzer and GC/MS; Promptly adopt online product analysis pattern, though use this online product analysis method have detection sensitivity high with characteristics fast, easily, quantitative accurately owing to not adopting internal standard method or external standard method to carry out; The analysis result of its product is qualitative often or semiquantitative, and it mainly is suitable for the product in the single temperature section is analyzed; In addition, analyze the sample introduction quantitative limitation owing to be heated, the on-line analysis method also is difficult to obtain comparatively all sidedly the research information of product, especially some micro-products.The research that the method for existing employing off-line is analyzed hot assay products.For example; 200910172481.3 Chinese patents of people such as Wang Hongbo invention; This method discloses a kind of elder generation and captured the thermogravimetric analysis product, adopted the method for thermal desorption and GC/MS technology off-line analysis then, though can be implemented in the interior analysis to volatility in the tobacco and half volatile compound and high-temperature split product of different temperatures section with capturing adsorption tube; But this method can not realize the product in the different temperatures section is carried out continual continuous collection; And owing to captured the influence of adsorption tube arresting efficiency, this method is difficult to also realize that the product in the same temperature section repeatedly effectively collects, and also can't adopt inside and outside mark method that product is carried out accurate quantitative test simultaneously; Therefore, its concrete application also receives very big restriction.
Summary of the invention:
For overcoming the defective of prior art; The object of the present invention is to provide a kind of simple in structure, easy to operate, good reproducibility; Can repeatedly effectively collect the corresponding product that the volatility in the different temperatures section in result of combustion of tobacco and the pyrolytic process and tar attitude product carry out in continual continuous collection and the same temperature section; And can realize product is carried out accurately qualitative, quantitative hot assay products gathering-device; Thereby for the tobacco scientific and technical personnel use thermal analyzer simulation cigarette burning condition, the formation mechanism of research result of combustion of tobacco process and flavor component and objectionable constituent provides a kind of good technological means.
Technical solution problem of the present invention adopts following technical scheme:
A kind of hot assay products gathering-device is provided with the polygonal nut of multiport, and one of them port is the gas stream inbound port, circumferentially is distributed with a plurality of gas stream outbound ports along said multiport polygonal nut; The gas stream inbound port of the polygonal nut of said multiport is communicated with the gas outlet end of the pyrolysis oven of thermal analyzer, and each gas stream outbound port of the polygonal nut of said multiport is connected with two-port valve and cambridge filter gatherer in turn; The gas of said cambridge filter gatherer flows into end and links to each other with two-port valve, and another endpiece of cambridge filter gatherer links to each other with on-line analysis mass spectrum, gas collection bag or solution drip catcher.
Design feature of the present invention also is:
The gas stream inbound port of the polygonal nut of said multiport and inside are that the inverse-T-shaped nut of a cavity bipass is connected through screw thread, and " O " shape elastic seal ring of inverse-T-shaped nut thread base portion forms sealing between inverse-T-shaped nut and the polygonal nut of multiport; Said inverse-T-shaped nut is connected with the flange of gas outlet end bottom inverse-T-shaped nut of the pyrolysis oven of thermal analyzer.
Compared with present technology, beneficial effect of the present invention is embodied in:
The present invention is simple in structure, easy to operate, favorable reproducibility; Using under the thermal analyzer simulation cigarette burning condition, can repeatedly effectively collect the corresponding product that the product in the different temperatures section in result of combustion of tobacco and the pyrolytic process carries out in continual continuous collection and the same temperature section; Adopt multiple collection modes such as cambridge filter gatherer, gas collection bag or solution drip catcher to combine; Both can analyze gaseous products in the hot analytic process; Also can study tar attitude product simultaneously; The collection method of this product can be carried out pre-service to product before chemical analysis, thereby can realize hot assay products is carried out qualitative and quantitative analysis accurately; In addition, can also be utilized in the line analysis mass spectrum gas-phase product is carried out on-line analysis.Therefore; The present invention has overcome the deficiency that prior art exists effectively; Can study carefully the formation mechanism of result of combustion of tobacco and pyrolytic process and flavor component and objectionable constituent for the tobacco scientific and technical personnel, thereby instruct the compound design and the lowering harm and decreasing coking of cigarette, a kind of good technical means are provided.The present invention also can be applicable to the collection and the research of the hot assay products of other organism.
Description of drawings:
The structural representation that Fig. 1 is connected with thermal analyzer for the present invention;
Fig. 2 is the polygonal nut cross-sectional view of multiport of the present invention;
Fig. 3 is the inverse-T-shaped nut master of a present invention TV structure synoptic diagram.
Fig. 4 is the GC/MS analyzing total ion flow graph that cambridge filter is collected product among the embodiment 1.
Fig. 5 is that heat is analyzed TG/DTG (thermogravimetric/differential thermogravimetric) curve among the embodiment 2.
Fig. 6 be among the embodiment 2 sample at the HPLC analysis result of 5 thermal weight loss stages, 5 kinds of carbonyls.
Fig. 7 is the GC/MS analyzing total ion flow graph that sample is collected product among the embodiment 2 at I temperature section cambridge filter.
Fig. 8 is the GC/MS analyzing total ion flow graph that sample is collected product among the embodiment 2 at II temperature section cambridge filter.
Fig. 9 is the GC/MS analyzing total ion flow graph that sample is collected product among the embodiment 2 at III temperature section cambridge filter.
Figure 10 is the GC/MS analyzing total ion flow graph that sample is collected product among the embodiment 2 at IV temperature section cambridge filter.
Figure 11 is the GC/MS analyzing total ion flow graph that sample is collected product among the embodiment 2 at V temperature section cambridge filter.
Label among the figure: the polygonal nut of 1 multiport, 1a gas stream inbound port, 1b gas stream outbound port, 2 inverse-T-shaped nuts; 2a " O " shape elastic seal ring, 2b flange, 3 two-port valves, 4 cambridge filter gatherers; 5 on-line analysis mass spectrums, 6 gas collection bags, 7 solution drip catchers, the pyrolysis oven of 8 thermal analyzers.
Below pass through embodiment, and combine accompanying drawing that the present invention is described further.
Embodiment:
Embodiment: Fig. 1, shown in Figure 2, a port of the polygonal nut 1 of multiport is gas stream inbound port 1a, along a plurality of gas stream outbound port 1b of circumferentially being distributed with of the polygonal nut 1 of multiport; The gas stream inbound port 1a of the polygonal nut 1 of multiport is communicated with the gas outlet end of the pyrolysis oven 8 of thermal analyzer, and each gas stream outbound port 1b of the polygonal nut 1 of said multiport is connected with two-port valve 3 and cambridge filter gatherer 4 in turn; The gas of said cambridge filter gatherer 4 flows into end and links to each other with two-port valve 3, and another endpiece of cambridge filter gatherer 4 links to each other with on-line analysis mass spectrum 5, gas collection bag 6 or solution drip catcher 7.
Fig. 1, shown in Figure 3; In specifically being provided with; The gas stream inbound port 1a of the polygonal nut 1 of multiport and inside are that the inverse-T-shaped nut 2 of a cavity bipass is connected through screw thread; And " O " shape elastic seal ring 2a of inverse-T-shaped nut 2 threaded base portion forms sealing between inverse-T-shaped nut 2 and the polygonal nut 1 of multiport, thereby guaranteed to connect can not leak here; The gas outlet end of inverse-T-shaped nut 2 and the pyrolysis oven 8 of thermal analyzer is connected through the flange 2b of inverse-T-shaped nut 2 bottoms, and is provided with elastic sealing strip at the joint face of flange 2b, thereby has guaranteed that this junction also can not leak gas.
Thermal analyzer used in the present invention is the anti-STA449C simultaneous thermal analysis appearance of speeding, and the gas vent of its pyrolysis oven 8 also can be communicated with the gas stream inbound port 1a of the polygonal nut of multiport with gastight any way.
Thermal analyzer used in the present invention has two sample holders, can measure TG and DSC curve simultaneously, also can measure the TG curve separately.When needs obtain heat analysis TG and DSC curve simultaneously, select TG/DSC sample holder and maximum tobacco sample amount to be about the small sample crucible of 30mg; When only needing to obtain heat analysis TG curve, select TG sample holder and maximum tobacco sample amount to be about the large sample crucible of 140mg.
During experiment, press earlier Fig. 1 assembling, connect instrument, accurately take by weighing the crucible that an amount of offal sample places thermal analyzer then, thermoanalytical initial temperature, heating rate are set, and the blending ratio and the flow of nitrogen/oxygen carrier gas, experiment begun.During product in needs are collected whole experiment initial temperature scope; Open a two-port valve 3; Close remaining two-port valve 3, the tar attitude product that tobacco sample burning this moment, pyrolysis produce and gas-phase product are collected through the cambridge filter gatherer 4 that links to each other with this two-port valve of opening 3 and gas collection bag 6 or solution drip catcher 7 respectively; During product in needs are collected the different temperatures section continuously; At first open a two-port valve 3; Close remaining two-port valve 3, the temperature of treating pyrolysis oven 8 arrives next product when collecting the initial temperature of temperature section, closes the previous two-port valve of having opened 3; Open next two-port valve 3 simultaneously, the product in the different temperatures section can be collected with gas collection bag 6 or solution drip catcher 7 through the cambridge filter gatherer 4 that is connected with the corresponding two-port valve of opening 3 like this.In above-mentioned experiment, gas-phase product also can directly be analyzed with on-line analysis mass spectrum 5.In addition, experiment can also be carried out repeatedly repetitive operation under the condition of not taking cambridge filter gatherer 4, gas collection bag 6 or solution drip catcher 7 away; Also can replace new cambridge filter, and the different cambridge filters under the repeatedly repetitive operation condition are put into the same extraction flask of relevant temperature section.Can collect product more like this, thereby obtain the research information of product, especially some micro-products more all sidedly.
After thermal analysis experiment finished, the tar attitude product that cambridge filter gatherer 4 is collected detected with GC/MS or other analytical instrument after in extraction, adding, marking and concentrate; The product that gas collection bag 6 is collected can be used instrument detecting such as mass spectrum, gas chromatography, FFIR; The product that solution drip catcher 7 is collected can be with instrumental analysis such as chromatograms.
Embodiment 1:
Open a two-port valve, close remaining two-port valve, hot assay products is adopted single channel and is collected.Select the TG sample holder, take by weighing the crucible that 100mg tobacco leaf powdered sample places thermal analyzer.Heat is analyzed heating rate and is set to: 20 ℃/min; Temperature range is set to: room temperature～1000 ℃; Carrier gas flux is set to: total flow is 100mL/min, and nitrogen/oxygen is 9/1.Beginning to heat up experimentizes, and tar attitude product is collected with cambridge filter in the hot analytic process, the direct emptying of gas-phase product.Heat analysis is taken off cambridge filter after finishing, and it is positioned in the Erlenmeyer flask of a 100mL.Then, the new filter disc of in the cambridge filter gatherer, packing into repeats twice of above-mentioned experiment; Latter two cambridge filter is put into the Erlenmeyer flask that previous cambridge filter is housed; In Erlenmeyer flask, add the 50mL methylene chloride, behind the vibration 30min, pipette the 40mL extract and place concentrated bottle; And add 0.5mL concentration be γ-certain herbaceous plants with big flowers lactone of 1.1mg/mL as interior mark, then extract is concentrated into 1mL and carries out GC/MS and analyze.
GC/MS (Agilent 6890GC/5973MSD) analysis condition is: chromatographic column is DB-35MS capillary chromatographic column (30m * 0.25mm * 0.25 μ m); 250 ℃ of injector temperatures, 280 ℃ of MSD transmission line temperature; Helium is as carrier gas, and flow is 1.0mL/min; Split sampling not, sample size 2.0 μ L; Adopt temperature programme, 40 ℃ of initial temperatures keep 2min, and the speed with 4 ℃/min rises to 250 ℃ then, keeps 5min again; 230 ℃ of ion gun (EI) temperature; 150 ℃ of quadrupole rod temperature; Electron-multiplier voltage 70eV; Sweep limit is 35～500m/z.
The product analysis result is referring to Fig. 4.
Before carrying out product collection experiment; Separately tobacco sample is carried out heat analysis earlier, select the TG sample holder, take by weighing the crucible that 120mg tobacco leaf powdered sample places thermal analyzer; The thermal analysis experiment condition is with embodiment 1, and heat is analyzed TG/DTG (thermogravimetric/differential thermogravimetric) curve referring to Fig. 5.DTG from Fig. 5 (differential thermogravimetric) curve can clearly be seen that this tobacco sample has mainly experienced 5 tangible thermal weight loss stages in combustion process, and the temperature range in I stage is: room temperature～140 ℃; The temperature range in II stage is: 140 ℃～240 ℃; The temperature range in III stage is: 240 ℃～370 ℃; The temperature range in IV stage is: 370 ℃～730 ℃; The temperature range in V stage is: 730 ℃～1000 ℃.
Then, carry out the collection experiment of product, hot analysis condition adopts 5 channel modes to 5 thermal weight loss stages in the tobacco sample combustion process with separately tobacco sample to be carried out thermoanalytical experiment condition identical, and the interior product of promptly above-mentioned 5 temperature sections is collected continuously.Except collecting tar attitude product; 5 kinds of volatile carbonyl compounds such as the formaldehyde in the gas-phase product, acetaldehyde, acetone, acryl aldehyde and propionic aldehyde adopt 20mL 2; Perchloric acid/acetonitrile solution (3.396g2 of 4-dinitrophenylhydrazine; 4-dinitrophenylhydrazine+1L acetonitrile+1.85mL perchloric acid, acetonitrile is settled to 2L) collect.After thermal analysis experiment finishes for the first time, take off the solution drip catcher, and analyze with high performance liquid chromatography (HPLC); Prepare the mixed mark solution of above-mentioned 5 kinds of carbonyls of a series of variable concentrations before analyzing earlier, the metric works curve adopts external standard method quantitative, and retention time is qualitative.
HPLC (Agilent 1100) analysis condition is: chromatographic column is DIONEX
Explosives E2 post (4.6mm * 250mm, 5 μ m); Column temperature is 30 ℃, and column flow rate is 1.0mL/min; Mobile phase A is a water, and Mobile phase B is an acetonitrile; Gradient elution, 0～20min, the volume fraction of A is 50%, 20～25min; The volume fraction of A is by 50% to 60%, 25～30min, and the volume fraction of A is 60%, 30～35min; The volume fraction of A is by 60% to 80%, 35～40min, and the volume fraction of A is to 90%, 40～41min by 80%; The volume fraction of A is by 90% to 50%, 41～45min, and the volume fraction of A is 50%; Sample size is 10 μ L; UV-detector, the detection wavelength is 325nm.
In 5 thermal weight loss stages, promptly the HPLC analysis result of 5 interior carbonyls of temperature section is referring to Fig. 6.
Meanwhile; Under the condition of declining the cambridge filter that renews, repeat above-mentioned experiment four times, the direct emptying of gas-phase product this moment; The pre-treating method of the tar attitude product that cambridge filter is collected and analysis condition are with embodiment 1, and the GC/MS analysis result is referring to Fig. 7, Fig. 8, Fig. 9, Figure 10 and Figure 11.
Therefore; Hot assay products gathering-device provided by the present invention; Can use under the thermal analyzer simulation cigarette burning condition; Can either carry out continual continuous collection to tar attitude product in the different temperatures section in result of combustion of tobacco, the pyrolytic process and gas-phase product, also can repeatedly effectively collect, can also realize accurate quantitative test simultaneously hot assay products to the corresponding product in the same temperature section; Thereby the formation mechanism for the tobacco scientific and technical personnel study result of combustion of tobacco process and flavor component and objectionable constituent provides a kind of effective technical and means.
Claims (2)
1. a hot assay products gathering-device is characterized in that being provided with the polygonal nut of multiport (1), and one of them port is gas stream inbound port (1a), circumferentially is distributed with a plurality of gas stream outbound ports (1b) along the polygonal nut of said multiport (1); The gas stream inbound port (1a) of the polygonal nut of said multiport (1) is communicated with the gas outlet end of the pyrolysis oven (8) of thermal analyzer, and each gas stream outbound port (1b) of the polygonal nut of said multiport (1) is connected with two-port valve (3) and cambridge filter gatherer (4) in turn; The gas of said cambridge filter gatherer (4) flows into end and links to each other with two-port valve (3), and another endpiece of cambridge filter gatherer (4) links to each other with on-line analysis mass spectrum (5), gas collection bag (6) or solution drip catcher (7).
2. a kind of hot assay products gathering-device according to claim 1; The gas stream inbound port (1a) that it is characterized in that the polygonal nut of said multiport (1) and inside are that the inverse-T-shaped nut (2) of a cavity bipass is connected through screw thread, and " O " shape elastic seal ring (2a) of inverse-T-shaped nut (2) threaded base portion forms sealing between inverse-T-shaped nut (2) and the polygonal nut of multiport (1); Said inverse-T-shaped nut (2) is connected with the flange (2b) of gas outlet end bottom inverse-T-shaped nut (2) of the pyrolysis oven (8) of thermal analyzer.
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| CN2010102817362A CN101995418B (en) | 2010-09-08 | 2010-09-08 | Gathering device for thermoanalysis product |
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| CN2010102817362A CN101995418B (en) | 2010-09-08 | 2010-09-08 | Gathering device for thermoanalysis product |
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| CN101995418B true CN101995418B (en) | 2012-05-09 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102830130A (en) * | 2011-06-16 | 2012-12-19 | 中国科学院上海硅酸盐研究所 | Method for quantitatively determining CO2 gas emitted from thermal analysis-mass spectrometry system |
| CN110967365A (en) * | 2019-12-17 | 2020-04-07 | 河北科技大学 | Method for analyzing pyrolysis kinetics of metal organic framework material based on combination of thermal analysis and mass spectrometry |
| 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 |
| CN113109483B (en) * | 2021-05-07 | 2023-05-16 | 上海烟草集团有限责任公司 | Analysis method of pyrolysis aroma components of latent aroma type aroma raw materials for cigarettes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DK84395A (en) * | 1995-07-18 | 1997-01-19 | Franz Floto | Apparatus for measuring water potential |
| CN101692032A (en) * | 2009-10-19 | 2010-04-07 | 中国烟草总公司郑州烟草研究院 | Method and device for off-line analysis of products generated by simulated combustion of cigarettes |
| CN201811930U (en) * | 2010-09-08 | 2011-04-27 | 安徽中烟工业公司 | Device for collecting thermal analysis product |
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2010
- 2010-09-08 CN CN2010102817362A patent/CN101995418B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DK84395A (en) * | 1995-07-18 | 1997-01-19 | Franz Floto | Apparatus for measuring water potential |
| CN101692032A (en) * | 2009-10-19 | 2010-04-07 | 中国烟草总公司郑州烟草研究院 | Method and device for off-line analysis of products generated by simulated combustion of cigarettes |
| CN201811930U (en) * | 2010-09-08 | 2011-04-27 | 安徽中烟工业公司 | Device for collecting thermal analysis product |
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Address after: 230088 No. 606 Huangshan Road, Hefei High-tech Zone, Anhui Province Patentee after: China Tabacco Anhui Industrial Co., Ltd. Address before: 230088 Mount Huangshan Road, Anhui, China, No. 606, No. Patentee before: China Tobacco Anhui Industrial Corporation |
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