CN103487534A - Automatic single drop micro-extraction apparatus for trapping thermogravimetric escaping gas - Google Patents
Automatic single drop micro-extraction apparatus for trapping thermogravimetric escaping gas Download PDFInfo
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- CN103487534A CN103487534A CN201310472199.3A CN201310472199A CN103487534A CN 103487534 A CN103487534 A CN 103487534A CN 201310472199 A CN201310472199 A CN 201310472199A CN 103487534 A CN103487534 A CN 103487534A
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Abstract
The invention discloses an automatic single drop micro-extraction apparatus for trapping a thermogravimetric escaping gas. The apparatus is formed by an L-shaped adapter provided with a heating device, an automatic needle pump, a microinjector, an infrared emitter, an infrared receiver and a controller; a ceramic outlet at the tail end of a thermogravimetric analyzer furnace body is connected with the L-shaped adapter; the infrared emitter and the infrared receiver are arranged in the L-shaped adapter; the automatic needle pump is arranged over a gas outlet of the L-shaped adapter, and the microinjector is arranged in the automatic needle pump; and the controller is connected with the infrared emitter, the infrared receiver and the automatic needle pump, and a sample disc and a reference disc are arranged in the thermogravimetric analyzer furnace body connected with the apparatus. A substance for analysis on the thermogravimetric analyzer sample disc undergoes programmed heating for gradual thermal decomposition, and the hermogravimetric escaping gas of the substance for analysis is carried to a furnace body outlet by a carrying gas and is automatically trapped by micro drops of a specific extract liquid, so the composition of the escaping gas is qualitatively and quantitatively analyzed by using a gas chromatography-mass spectrometry instrument. There is no artificial intervention, so the good reappearance of each experiment can be guaranteed.
Description
Technical field
The present invention relates to a kind of analytical chemistry pretreatment technology, specifically a kind ofly for the thermogravimetric emergent gas, trap automatic single liquid drop micro-extractor.
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.Though the Py-GC/MS coupling technique has been widely used in the splitting mechanism of Main chemical component etc. in monomeric additive, tobacco, the research of metastatic rule, but when the Pintsch process behavior for analytic sample, because amount of samples is very little, and can only the cracking information of sampling under specified temp point, its result can not reflect the continuous situation of change of sample effusion product in whole temperature-rise period.
Thermogravimetric analyzer (TGA) is a kind of a kind of hot analysis classes instrument that utilizes thermogravimetry (TG) detection material temperature-mass change relation.The advantages such as that TGA has is easy and simple to handle, accuracy and highly sensitive, micro-ization of sample, be widely used in the numerous areas such as inorganic, organic, chemical industry, food.TGA heats and can simulate the oxygen-free environment in cigarette combustion cone under inert atmosphere, but the combustion process of Temperature Programmed Processes partial simulation cigarette, and yet can't overflow to thermogravimetric, component is trapped and qualitative and quantitative analysis.
Single drop micro-extraction (SDME) technology is a kind of novel Sample Pretreatment Technique grown up on the liquid-liquid extraction basis in recent years.It is that an extraction solvent is suspended to the extracting head tip, then is dipped in sample solution or is suspended from the sample headroom, makes analyte be transferred to the technology of organic phase (extraction solvent) from water or gas phase.Because SDME is the preconditioning technique that utilizes distribution principle to carry out, therefore can solve well the supersaturation problem in extraction process, there is in addition enrichment times high, the advantage such as detectability is low.But SDME Technology Need manual operation usually, and each micro-droplet size formed is inconsistent, thereby the reappearance of testing result is had to considerable influence.
Summary of the invention
The object of the invention is to overcome that above-mentioned existing Py-GC/MS and thermogravimetric analyzer can not trap pyrolysis effusion product effectively and the shortcoming of qualitative and quantitative analysis, provide a kind of automatic single liquid drop micro-extractor that is applied to the trapping of thermogravimetric emergent gas, to realize the qualitative and quantitative analysis to the emergent gas component.
The present invention is achieved through the following technical solutions: automatic single liquid drop micro-extractor of the present invention consists of the L-type adapter with heating arrangement, automatic pin pump, micro syringe, infrared transmitter, infrared remote receiver and controller; The Ceramic Export of thermogravimetric analyzer body of heater end is connected with the L-type adapter; L-type adapter built-in infrared transmitter and infrared remote receiver; Automatically the pin pump is placed in the top of L-type adapter exhausr port, and automatically in the pin pump, micro syringe is installed; Controller connects infrared transmitter and infrared remote receiver and automatic pin pump, the built-in sample disc of thermogravimetric analyzer body of heater and the reference dish that are connected with this device.
Analysans is placed on the sample disc of thermogravimetric analyzer, in the specific gas atmosphere, (nitrogen oxygen atmosphere of inert gas or certain proportioning) carries out temperature programme, the volatile matter discharged after the material decomposes (effusion gas) flows out through the outlet of thermogravimetric analyzer body of heater end ceramic pipe, through the L-type adapter, upwards derive, be suspended from micro-drop trapping of micro syringe syringe needle and concentrate, owing to by infrared beam, controlling droplet size, extraction process can complete automatically.Sample carries out pyrolysis under thermogravimetric analyzer temperature programme condition, and the effusion component is to be driven and discharged from escape hole by carrier gas.After having trapped, collect micro-drop and carry out qualitative and quantitative analysis, and, according to the character that traps material, choose corresponding extract the residual component in the L-type adapter is carried out to wash-out.
The extract that single drop micro-extraction is used is chosen according to the character of the material that is captured.
The nitrogen oxygen atmosphere that described specific gas atmosphere is inert gas or certain proportioning.
Analysans is placed on the sample disc of thermogravimetric analyzer, in the specific gas atmosphere, (nitrogen oxygen atmosphere of inert gas or certain proportioning) carries out temperature programme, the volatile matter discharged after the material decomposes (effusion gas) flows out through thermogravimetric analyzer end ceramic pipe, after the L-type adapter is upwards derived, be suspended from micro-drop trapping of micro syringe syringe needle and concentrate, owing to by infrared beam, controlling droplet size, extraction process can complete automatically.
Device of the present invention has following characteristics: automatically complete micro-drop extraction process 1..2. this combined apparatus, can be used for the quantitative examination of volatile matter in pipe tobacco thermogravimetric emergent gas, for the research that reduces volatile phenol material growing amount in 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 be detected, and with the combined apparatus (as Py-GC/MS) of existing analytical instrument, compare, and have obvious advantage.
The present invention can reduce the error of manual operation for the automatic single liquid drop micro-extractor of thermogravimetric effusion gas trapping, micro-droplet size that each extraction process is used is consistent, guarantee that each experiment all has good reappearance, improve the arresting efficiency of volatile matter in the thermogravimetric emergent gas.
The accompanying drawing explanation
Fig. 1 is the automatic single liquid drop micro-extractor structural representation for the trapping of thermogravimetric effusion gas of the present invention.
Sequence number in Fig. 1: 1-sample disc; 2-reference dish; 3-thermogravimetric analyzer body of heater; 4-L-type adapter; 5-L-type adapter heating unit; 6-glass enclosure tube; 7-infrared transmitter; 8-infrared remote receiver; 9-infrared beam, the automatic pin pump of 10-, 11-micro syringe, 12-controller.
Embodiment
Below in conjunction with embodiment and accompanying drawing, automatic single liquid drop micro-extractor of the present invention is further described:
Automatic single liquid drop micro-extractor of the present invention is by L-type adapter 4, adapter heating unit 5, glass enclosure tube 6, infrared transmitter 7, infrared remote receiver 8, automatic pin pump 10, micro syringe 11, controller 12.The built-in sample disc 1 of thermogravimetric analyzer body of heater and reference dish 2; The thermogravimetric analyzer body of heater is connected with L-type adapter 4, L-type adapter built-in infrared transmitter 7 and infrared remote receiver 8; Automatically pin pump 10 is placed in the top of L-type adapter exhausr port, and pin pump needle point is positioned at the position of exhausr port top 0.5cm automatically; Controller 12 connects infrared transmitter 7, infrared remote receiver 8 and automatic pin pump 10.
Described specific gas atmosphere is helium, nitrogen or nitrogen oxygen atmosphere.
The present invention traps the volatile matter of overflowing in the thermogravimetric Temperature Programmed Processes with automatic single liquid drop micro-extractor.At first connect the L-type adapter in thermogravimetric analyzer body of heater exit, thermogravimetric analyzer body of heater exit ceramic pipe is drawn, junction is sealed with the graphite pressure ring.Then connect successively glass enclosure tube, pin pump, infrared transmitter, infrared remote receiver, controller etc.After the thermogravimetric air escape goes out, be suspended from micro-extraction drop on syringe needle and extract concentratedly, with this, trap the volatile matter in the thermogravimetric emergent gas.
Its L-type adapter end is equipped with a glass enclosure tube, to intercept the impact of extraneous air-flow on thermogravimetric effusion component.Support is installed with locking pin pump, infrared transmitter and infrared remote receiver in thermogravimetric analyzer body of heater exit, and can makes it vertical and move left and right, be convenient to the adjustment of micro-extraction drop and infrared beam position.Promote micro syringe 11 by automatic pin pump, make needle point hang a full extraction drop and, under not falling, now droplet size is about 10 μ L.Adjust the infrared beam position simultaneously, make it tangent with the drop outer rim.After component gas is discharged, be suspended in immediately the drop extraction condensation of exhausr port top micro syringe needle point, continuous purging due to the thermogravimetric carrier gas can make the solvent evaporation cause droplet size to reduce simultaneously, automatically the pin pump starts voluntarily, promote micro syringe and discharge extract, make drop again reach full state, stop action after tangent to infrared beam and drop outer rim, and so forth.
The drop that collection completes extraction carries out compartment analysis at the laggard high performance liquid chromatography of filtering membrane or gas chromatography/mass spectrometry.
For example: adopt device of the present invention,, under nitrogen atmosphere the simple aldehydes matter in tobacco sample pyrolysis effusion gas is trapped and quantitative and qualitative analysis research in conjunction with high performance liquid chromatography.Concrete steps are as follows:
Get 20 cigarette, pipe tobacco is taken out, be placed in 40 ± 1 ℃ of baking oven inner dryings and pulverized 40 mesh sieves after 2 hours, standby in the valve bag of packing into.
Before experiment, first thermogravimetric analyzer is warming up under certain air velocity to 1000 ℃ and keep 10 min, to get rid of the impurity in body of heater.After under furnace body temperature is down to room temperature, accurately take quantitative tobacco sample and be placed on the sample disc in the thermogravimetric analyzer body of heater, from room temperature, under 300 mL/min nitrogen flows, with the heating rate of 10 ℃/min, be warming up to 600 ℃.
Along with the rising of temperature, the pyrolytic process of pipe tobacco has roughly experienced 4 stages: from room temperature～125 ℃, 125～220 ℃, 220～390 ℃, 390～600 ℃, when temperature surpasses 600 ℃, the thermal weight loss of pipe tobacco almost no longer changes.The thermal weight loss process that has obtained thus this tobacco sample mainly occurs between room temperature～600 ℃.In Temperature Programmed Processes, device of the present invention is trapped seven kinds of simple aldehydes matters in the pipe tobacco emergent gas.Form the aqueous acetic acid that solution that single drop is used is 1%.After having trapped, drop is proceeded to the chromatogram bottle, utilize high performance liquid chromatography to be analyzed extraction solution.
The present invention is existing applies to the simulation of tobacco pyrolytical condition by it, and the while, in conjunction with the capturing device of designed, designed, is trapped and qualitative and quantitative analysis the material in the thermogravimetric emergent gas, thereby has made up the deficiency of Py-GC/MS.In addition, this capturing device also has advantages of that the secondary reaction of minimizing occurs, thereby it has significant advantage aspect mechanism of research material.
Claims (1)
1. the automatic single liquid drop micro-extractor for the trapping of thermogravimetric effusion gas, is characterized in that: the L-type adapter with heating arrangement, automatic pin pump, micro syringe, infrared transmitter, infrared remote receiver and controller, consist of; The Ceramic Export of thermogravimetric analyzer body of heater end is connected with the L-type adapter; L-type adapter built-in infrared transmitter and infrared remote receiver; Automatically the pin pump is placed in the top of L-type adapter exhausr port, and automatically in the pin pump, micro syringe is installed; Controller connects infrared transmitter and infrared remote receiver and automatic pin pump, the built-in sample disc of thermogravimetric analyzer body of heater and the reference dish that are connected with this device.
2. according to claim 1 for the automatic single liquid drop micro-extractor of thermogravimetric effusion gas trapping, it is characterized in that: the outer ancient piece of jade, round, flat and with a hole in its centre of L-type adapter is heating unit.
3. according to claim 1 for the automatic single liquid drop micro-extractor of thermogravimetric effusion gas trapping, it is characterized in that: there is a glass enclosure tube L-type adapter upper end.
4. according to claim 1 for the automatic single liquid drop micro-extractor of thermogravimetric effusion gas trapping, it is characterized in that: in thermogravimetric analyzer body of heater exit, the fixedly support of micro syringe, infrared transmitter and infrared remote receiver is installed.
5. according to claim 1 for the automatic single liquid drop micro-extractor of thermogravimetric effusion gas trapping, it is characterized in that: the needle point of pin pump is positioned at the position of exhausr port top 0.5cm automatically.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237058A (en) * | 2014-09-23 | 2014-12-24 | 中国科学技术大学 | Thermogravimetric molecular beam mass spectrum combined device |
| CN106248469A (en) * | 2016-10-31 | 2016-12-21 | 钟曼匀 | A kind of continuous micro-extraction device of drop being automatically replenished collection drop and extracting process |
| CN106345751A (en) * | 2015-07-14 | 2017-01-25 | 中国石油天然气股份有限公司 | Platinum sample plate cleaning method |
| CN106442746A (en) * | 2016-06-17 | 2017-02-22 | 中检集团南方电子产品测试（深圳）股份有限公司 | Method for measuring content of red phosphorus in polymer |
| 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 |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
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| CN202614732U (en) * | 2012-06-04 | 2012-12-19 | 云南烟草科学研究院 | On-line gathering and analyzing device for polycyclic aromatic hydrocarbon in thermal cracking products |
| CN203551531U (en) * | 2013-10-11 | 2014-04-16 | 云南烟草科学研究院 | Automatic single-drop microextraction device for trapping TGA (Thermal Gravity Analysis) escaping gas |
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| WO2011031005A2 (en) * | 2009-09-08 | 2011-03-17 | Snu R & Db Foundation | Single drop microextraction method combined with capillary electrophoresis-mass spectrometry |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237058A (en) * | 2014-09-23 | 2014-12-24 | 中国科学技术大学 | Thermogravimetric molecular beam mass spectrum combined device |
| CN106345751A (en) * | 2015-07-14 | 2017-01-25 | 中国石油天然气股份有限公司 | Platinum sample plate cleaning method |
| CN106345751B (en) * | 2015-07-14 | 2018-11-16 | 中国石油天然气股份有限公司 | A kind of method for cleaning of platinum sample disc |
| CN106442746A (en) * | 2016-06-17 | 2017-02-22 | 中检集团南方电子产品测试（深圳）股份有限公司 | Method for measuring content of red phosphorus in polymer |
| CN106442746B (en) * | 2016-06-17 | 2017-08-08 | 中检集团南方电子产品测试（深圳）股份有限公司 | A kind of method of red phosphorus content in test polymer |
| CN106248469A (en) * | 2016-10-31 | 2016-12-21 | 钟曼匀 | A kind of continuous micro-extraction device of drop being automatically replenished collection drop and extracting process |
| CN106248469B (en) * | 2016-10-31 | 2024-04-02 | 钟曼匀 | Liquid drop continuous micro-extraction device capable of automatically supplementing and collecting liquid drops and extraction method |
| 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 |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
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| CN103487534B (en) | 2014-12-31 |
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