CN102507270B - Thermogravimetric analyzer and Cambridge filter-absorption bottle combination apparatus and emergent gas gathering method - Google Patents
Thermogravimetric analyzer and Cambridge filter-absorption bottle combination apparatus and emergent gas gathering method Download PDFInfo
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- CN102507270B CN102507270B CN 201110344613 CN201110344613A CN102507270B CN 102507270 B CN102507270 B CN 102507270B CN 201110344613 CN201110344613 CN 201110344613 CN 201110344613 A CN201110344613 A CN 201110344613A CN 102507270 B CN102507270 B CN 102507270B
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Abstract
The invention discloses a thermogravimetric analyzer and Cambridge filter-absorption bottle combination apparatus and a usage method thereof, which is characterized in that: a substance is placed in a sample crucible of the thermogravimetric analyzer, and is heated with temperature programming in inertia atmosphere, and the substance releases volatile materials after thermal decomposition; the volatile materials are gathered by the Cambridge filter, and then secondary gathering is carried out by the absorption liquid. The invention has the following three characteristics: 1. different gathering modes have different gathering effects on different volatile materials, and two gathering modes are used in series, thereby compensating the defect that a single gathering mode can not gather volatile materials completely; 2. the combination apparatus can be used for semi-quantification research for volatile materials in cut tobacco thermogravimetric emergent gas, thereby providing a new research method for researching the reduction of the generation amount of volatile materials in cigarette gas; 3. the invention has the advantages of simple apparatus and convenient operation, and the extract or absorption liquid after treatment can be detected by different analysis apparatuses.
Description
Technical field
The present invention relates to a kind of analytical chemistry pre-treatment means.Specifically be to use cambridge filter-absorption bottle combined apparatus to capture the thermogravimetric emergent gas, to realize that the volatile matter in the material pyrolysis emergent gas is carried out the quantitative and semi-quantitative analysis.
Technical background
At present, in the various technology to the cigarette burning process simulation, comparatively typical a kind of is online pyrolysis gas chromatograph/mass spectrum (Py-GC/MS) coupling technique.Online pyrolysis gas chromatograph/mass spectrum (Py-GC/MS) is though coupling technique has been widely used in the splitting mechanism of Main chemical component in monomeric additive, the tobacco etc., the research of metastatic rule, but when the Pintsch process behavior of thermal cracking instrument analytic sample, because amount of samples is very little, and can only the cracking information of sampling under specified temp point, thermal cracking instrument analysis result can not reflect the continuous situation of change of sample effusion product in whole temperature-rise period.
Thermogravimetric analyzer is a kind of a kind of thermoanalysis technology of measuring sample quality and temperature variation relation under temperature programme, have that instrumentation is easy fast, the advantages such as accuracy and highly sensitive, micro-ization of sample, be widely used in the numerous areas such as inorganic, organic, chemical industry, food.Thermogravimetric analyzer heats the oxygen-free environment that can simulate cigarette burning under inert atmosphere, but the Temperature Programmed Processes combustion process of partial simulation cigarette then.
Summary of the invention
The object of the invention is to overcome above-mentioned existing thermogravimetric analyzer and coupling technique thereof can not carry out compartment analysis effectively to pyrolysis effusion product problem, invent a kind of with cambridge filter-absorption bottle combined apparatus, and with the capture of this application of installation in the thermogravimetric emergent gas, realize the material in the emergent gas is carried out the quantitative and semi-quantitative analysis.
The present invention also aims to, improve the arresting efficiency of volatile matter in the thermogravimetric emergent gas.Cambridge filter has Smoke Particulate and captures preferably effect, and absorption liquid then has the flue gas gas gas-phase objects and captures preferably effect, with the use that is together in series of cambridge filter and absorption bottle, can capture the volatile matter in the thermogravimetric effusion gas comprehensively.
The present invention also aims to, the material after the capture can adopt different instruments to analyze for its different character, compares with the combined apparatus (such as Py-GC/MS) that adopts intrinsic analytical instrument, has obvious advantage.
The present invention can be achieved through the following technical solutions: a kind of thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus, it is characterized in that: the outside control temperature unit (4) that described device comprises thermogravimetric analyzer and carries, the carrier gas flux meter, glass tube (5), cambridge filter unit (6), absorption bottle (7), connect first a glass tube (5) in the exit of thermogravimetric analyzer body of heater, so that ceramic pipe is drawn, the other end at glass tube (5) is connected to a cambridge filter unit (6) and an absorption bottle (7) successively, form cascaded structure cambridge filter-absorption bottle combined apparatus, wherein, cambridge filter unit (6) is cambridge filter or 1/4 cambridge filter that diameter is 44mm of 10mm by straightening the footpath in the middle of two microsyringe housings, and two ends clamp two housings with iron clamp and consist of.
The absorption liquid (8) that uses in the described absorption bottle (7) is then selected according to the character of the material that is captured.
Be positioned on the thermogravimetric platinum crucible specimen holder (3) in the thermogravimetric analyzer intending detection material, under inert atmosphere, carry out the temperature programme cracking, connect first a glass tube (5) in the body of heater exit of thermogravimetric analyzer, so that ceramic pipe is drawn, the other end at glass tube (5) sequentially connects a cambridge filter unit (6) and an absorption bottle (7), the cambridge filter that formation is connected in series-absorption liquid coupling structure, intend the volatile matter that the detection material decomposes discharges, after the process cambridge filter once captures, carrying out secondary by absorption liquid again captures, capture simultaneously the volatile matter in the thermogravimetric emergent gas, and with the volatile matter in the captured gas, carry out conventional sense and divide folding, obtain accurate data.
Described inert atmosphere is nitrogen.
The purpose that adopts two kinds of Trapping ways series connection of cambridge filter and absorption liquid to use in thermogravimetric analysis of the present invention and cambridge filter-absorption bottle combined apparatus is: cambridge filter only has the granule phase substance in the flue gas and captures preferably effect, absorption liquid then has the volatile matter in the flue gas and captures preferably effect, so two kinds of Trapping ways are combined use, but Effective Raise arresting efficiency.
Apparatus of the present invention have following characteristics: 1. different Trapping ways to different volatile matter the capture effect different, two kinds of Trapping ways series connection are used, can remedy the defective that single Trapping ways can not capture fully to volatile matter.2. this combined apparatus also can be used for the sxemiquantitative research of volatile matter in the pipe tobacco thermogravimetric emergent gas, for the research that reduces the growing amount of volatile phenol material in the cigarette smoke provides new research method.3. apparatus of the present invention are simple, easy to operate, and extract or absorption liquid after processing can adopt different analytical instrument to detect.
Description of drawings
Fig. 1 is thermogravimetric analyzer of the present invention and cambridge filter-absorption bottle combined apparatus synoptic diagram.
Sequence number among Fig. 1: 1-carrier gas; The 2-balance arm; The 3-specimen holder; 4-body of heater heating unit; The 5-glass tube; 6-cambridge filter unit; The 7-absorption bottle; The 8-absorption liquid.
Fig. 2 is thermogravimetric, the difference quotient thermogravimetric curve figure of pipe tobacco.
Fig. 3 is the high-efficient liquid phase chromatogram of seven kinds of volatile phenol standard solution.
Fig. 4 is the HPLC spectrogram that absorption liquid captures seven kinds of volatile phenols in the pipe tobacco pyrolysis effusion product.
Fig. 5 is the HPLC spectrogram that cambridge filter captures seven kinds of volatile phenols in the pipe tobacco pyrolysis effusion product.
Fig. 6 is the GC//MS total ions chromatogram that absorption liquid captures cellulose pyrolysis effusion product.
Fig. 7 is the GC/MS total ions chromatogram that cambridge filter captures cellulose pyrolysis effusion product.
Embodiment
The present invention utilizes cambridge filter and two kinds of Trapping ways of absorption liquid to capture the volatile matter of overflowing in the thermogravimetric Temperature Programmed Processes.Thermogravimetric body of heater outlet heating tape temperature is regulated by the external temperature control module that thermal analyzer carries.At first connect a glass tube in the body of heater exit, body of heater exit ceramic pipe is drawn, the junction seals with the graphite pressure ring.Then with proofed sleeve glass tube, cambridge filter unit, series connection absorption bottle are linked to each other successively, capture volatile matter in the thermogravimetric emergent gas with this.
The inventive system comprises thermogravimetric analyzer, carrier gas flux meter, glass tube, cambridge filter unit, absorption bottle.Wherein, the cambridge filter cell formation is: straighten the footpath in the middle of two microsyringe housings and be the cambridge filter of 10mm or 1/4 cambridge filter that diameter is 44mm, two ends clamp two housings with iron clamp.The absorption liquid that fills in the absorption bottle is chosen according to the character of the material that is captured.
Described inert atmosphere is nitrogen.
Sample carries out pyrolysis under thermogravimetric analyzer temperature programme condition, the effusion component is to discharge from escape hole together under the carrier gas of carrier gas flux meter control drives.
The using method of the thermogravimetric analysis of sample pyrolysis behavior and cambridge filter-absorption bottle combined apparatus, its feature mainly comprises the following aspects:
Sample is put into the sample crucible of thermogravimetric analyzer, get the empty crucible of same model as reference.Set suitable experiment condition, comprising: heating rate, sample size, carrier gas flux etc.
In conjunction with material to be analyzed, select suitable absorption liquid, the aqueous acetic acid such as 1%, ethanol etc.
The glass tube of front, cambridge filter unit directly is inserted on the cambridge filter by proofed sleeve, is enriched on the proofed sleeve to avoid the volatile matter in the emergent gas.
After capture is finished, according to the character that captures material, choose corresponding extract cambridge filter and glass tube are carried out pre-treatment.
Get respectively that above-mentioned an amount of extract and absorption liquid are crossed the laggard liquid chromatography of film or gas chromatography/mass spectrometry is carried out compartment analysis.
The present invention is further described the thermogravimetric analyzer of foundation the present invention proposition and application and the embodiment of cambridge filter-absorption bottle combined apparatus below with reference to embodiment (accompanying drawing):
Embodiment 1: adopt thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus seven kinds of volatile phenol materials in the tobacco sample pyrolysis effusion gas to be captured and quantitative and semi-quantitative research under inert atmosphere in conjunction with high performance liquid chromatography.Concrete steps are as follows:
Get 20 cigarette, pipe tobacco is taken out, place 40 ± 1 ℃ of baking oven inner dryings to pulverize 40 mesh sieves after 2 hours, for subsequent use in the sealed bag of packing into.
Before the experiment, first thermogravimetric analyzer is warming up to 1000 ℃ and keep 10min under air velocity 300mL/min, to get rid of the impurity in the body of heater.After the sample crucible temperature is down to below the room temperature, accurately take by weighing the 32mg tobacco sample and put into thermogravimetric sample platinum crucible, from room temperature, under the 300mL/min nitrogen flow, be warming up to 600 ℃ with the heating rate of 10 ℃/min.
The heat analysis data that obtains as shown in Figure 2, can find out in conjunction with the TG among the figure and DTG curve, rising along with temperature, the pyrolytic process of pipe tobacco has roughly experienced 4 stages: from room temperature～125 ℃, 125～220 ℃, 220～390 ℃, 390～600 ℃, when temperature surpassed 600 ℃, the thermal weight loss of pipe tobacco almost no longer changed.The thermal weight loss process that has obtained thus this tobacco sample mainly occurs between room temperature～600 ℃, then utilizes thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus that seven kinds of volatile phenol materials in the pipe tobacco emergent gas are captured.
Cambridge filter among the present invention adopts the cambridge filter of the 44mm diameter of Britain Whatman company, during use it is divided into 4 five equilibriums, and the absorption liquid in the absorption bottle is the aqueous acetic acid of 12mL 1%.
After capture is finished, glass tube and the cambridge filter taking-up of cambridge filter device front end are placed the 25mL conical flask, pipette the aqueous acetic acid of 10mL 1% to conical flask with transfer pipet, with the cambridge filter submergence, ultrasonic 20min under room temperature, leave standstill 5min, get an amount of upper layer of extraction liquid and cross the liquid chromatography bottle of packing into behind the 0.45 μ m miillpore filter.Simultaneously capture there is the absorption liquid of volatile phenol material to shake up, got in right amount and to cross the chromatogram bottle of packing into behind the 0.45 μ m miillpore filter.
Utilize HPLC that the mixed mark solution that contains seven kinds of volatile phenol materials is analyzed, the result analyzes the solution in above two liquid chromatography bottles that obtain as shown in Figure 3 simultaneously, and the result as shown in Figure 4 and Figure 5.Comparison diagram 3,4,5 can find out, cambridge filter has preferably p-benzenediol, meta-benzenediol, these three kinds of materials of ortho-, meta-or p-benzenediol and captures, absorption liquid then the Pyrogentisinic Acid,, p-Cresol, ortho-, meta-or p-cresols have preferably and capture.Adopt the necessity of two kinds of Trapping ways in this explanation thermogravimetric analyzer and this combined apparatus of cambridge filter-absorption bottle.The p-benzenediol of 1-among the figure; The meta-benzenediol of 2-; The ortho-, meta-or p-benzenediol of 3-; 4-phenol; 5-pair, m-cresol; The ortho-, meta-or p-cresols of 6-.
Can be found out by Fig. 4 and Fig. 5, adopt this invention thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus, can carry out the simulated combustion experiment to cigarette, can realize seven kinds of volatile phenols in the pipe tobacco pyrolysis emergent gas are captured and the quantitative and semi-quantitative analysis.
Embodiment 2: adopt thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus in conjunction with GC/MS the pyrolysis behavior of cellulose pyrolysis effusion product to be studied.
Accurately take by weighing 30 ± 0.05mg cellulose sample and put into the thermogravimetric sample crucible, from room temperature, under the 400mL/min nitrogen flow, be warming up to 600 ℃ with the heating rate of 10 ℃/min.
After capture is finished, take off cambridge filter, with the cambridge filter cleaning glass window inside pipe wall that is moistened with in right amount ethanol, both are put into the GC/MS sample injection bottle simultaneously, add about 1.0mL ethanol (being as the criterion with the submergence cambridge filter), ultrasonic extraction 20min.
Absorption liquid is the ethanolic solution of 8mL.
The result is referring to GC/MS spectrogram (Fig. 6, Fig. 7)
The present invention is existing to apply to the simulation of tobacco pyrolytical condition with it, and the while captures and the quantitative and semi-quantitative analysis the material in the thermogravimetric emergent gas in conjunction with the capturing device of designed, designed, thereby has remedied the deficiency of Py-GC/MS.In addition, thermogravimetric analysis also has the advantage of the generation that has reduced secondary reaction, thereby it has significant advantage aspect mechanism of research material.
Claims (2)
1. a thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus, it is characterized in that: the outside control temperature unit (4) that described device comprises thermogravimetric analyzer and carries, the carrier gas flux meter, glass tube (5), cambridge filter unit (6), absorption bottle (7), connect first a glass tube (5) in the exit of thermogravimetric analyzer body of heater, so that ceramic pipe is drawn, the other end at glass tube (5) is connected to a cambridge filter unit (6) and an absorption bottle (7) successively, form cascaded structure cambridge filter-absorption bottle combined apparatus, wherein, cambridge filter unit (6) is cambridge filter or 1/4 cambridge filter that diameter is 44 mm of 10mm by straightening the footpath in the middle of two microsyringe housings, and two ends clamp two housings with iron clamp and consist of;
The absorption liquid (8) that uses in the described absorption bottle (7) is then selected according to the character of the material that is captured.
2. right to use requires 1 described thermogravimetric analyzer and cambridge filter-absorption bottle combined apparatus to capture the method for emergent gas, it is characterized in that: will intend detection material and be positioned on the thermogravimetric platinum crucible specimen holder (3) in the thermogravimetric analyzer, under inert atmosphere, carry out the temperature programme cracking, connect first a glass tube (5) in the body of heater exit of thermogravimetric analyzer, so that ceramic pipe is drawn, the other end at glass tube (5) sequentially connects a cambridge filter unit (6) and an absorption bottle (7), the cambridge filter that formation is connected in series-absorption liquid coupling structure, intend the volatile matter that the detection material decomposes discharges, after the process cambridge filter once captures, carrying out secondary by absorption liquid again captures, capture simultaneously the volatile matter in the thermogravimetric emergent gas, and with the volatile matter in the captured gas, carry out conventional sense and divide folding, obtain accurate data;
Described inert atmosphere is nitrogen.
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| US9629391B2 (en) * | 2013-08-08 | 2017-04-25 | R.J. Reynolds Tobacco Company | Tobacco-derived pyrolysis oil |
| CN103940602B (en) * | 2014-04-29 | 2017-03-08 | 云南中烟工业有限责任公司 | A kind of method that inspection electronic smoke atomizer is atomized uniformity |
| CN104215486B (en) * | 2014-09-12 | 2017-02-01 | 云南中烟工业有限责任公司 | Cigarette paper combustion product capturing method for biological detection |
| 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 |
| 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 |
| CN114618187B (en) * | 2022-02-28 | 2024-03-22 | 海南红塔卷烟有限责任公司 | Micro-bottle extraction device and method for thermogravimetric escaped matter analysis |
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| CN101692032B (en) * | 2009-10-19 | 2011-04-20 | 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 |
| CN201503368U (en) * | 2009-10-19 | 2010-06-09 | 中国烟草总公司郑州烟草研究院 | Simulating device for cigarette igniting and smoking |
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