CN202033333U - Gas-phase adsorption-desorption device having function of automatically analyzing injected samples - Google Patents
Gas-phase adsorption-desorption device having function of automatically analyzing injected samples Download PDFInfo
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- CN202033333U CN202033333U CN2011200619456U CN201120061945U CN202033333U CN 202033333 U CN202033333 U CN 202033333U CN 2011200619456 U CN2011200619456 U CN 2011200619456U CN 201120061945 U CN201120061945 U CN 201120061945U CN 202033333 U CN202033333 U CN 202033333U
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Abstract
The utility model discloses a gas-phase adsorption-desorption device having a function of automatically analyzing injected samples, which comprises a carrier gas supplying system, a dehydration deoxidizing tube, an electronic mass flow meter, an organic steam generator, a steam generator and a sample injection valve. A first gas passage of the sample injection valve is connected to an adsorption column, and the other end of the adsorption column is connected to a gas circuit conversion valve. The gas circuit conversion valve comprises a hand-actuated two-position valve, an electronic eight-position valve, a first passage and a second passage, wherein the first passage and the second passage extend from the two-position valve, and the two-position valve is connected to an outlet end of the adsorption column. The two-position gas circuit conversion valve is capable of realizing switching between continuous detection and intermittent detection, the eight-position valve is connected to the tail end of a gas circuit of the sample injection valve and used for collecting gas, the first passage is connected with a second gas passage of the sample injection valve, and the second passage is connected to a gas-phase chromatographic detector. A cold trap is additionally arranged outside the organic steam generator, and the adsorption column is arranged in a drying box. The gas-phase adsorption-desorption device is used for research of adsorption and degradation mechanism of volatile halohydrocarbon in mineral micropores and research of adsorption-desorption power of other matters as well after being slightly improved. Besides, the gas-phase adsorption-desorption device is easy to be mounted, convenient in operation and labor-saving.
Description
Technical field
The utility model relates to a kind of Gas Phase Adsorption-desorption apparatus that possesses the auto injection analytic function, relates to a kind of absorption-desorption device of volatility halogenated hydrocarbons in mineral matter micropore absorption degradation mechanism that be used for inquiring into especially.
Background technology
Along with developing rapidly of China's industrial and agricultural production, soil is subjected to the pollution of organic chemicals serious day by day, and to ecologic environment, food security and agricultural sustainable development constitute a serious threat.Wherein the volatility halogenated hydrocarbons is in chemical industry, metal-processing industry, and semiconductor manufacturing industry, the dry-cleaning industry, medicine and laboratory are used as organic solvent at large, become one of the pollutant the most widely that distributes in soil and the groundwater environment.This pollutant high volatility is slightly soluble in water, has toxicity, for the human and animal potential health threat is arranged.Migration and the destiny rule of research volatility halogenated hydrocarbons in soil and underground water has far-reaching directive significance to industrial and agricultural production management and environmental improvement.
Studies show that absorption is that soil and water-bearing zone medium are held the main mechanism that leaves organic pollutants, to the migration of organic contaminant, distribution plays a major role, and being influences its chemistry, the principal element of biological effectiveness.Soil and water-bearing zone medium are natural porosu solids, and along with the concern of people's environmental pollution problem, the pore texture of soil and micropore have become the new focus of research to the influence of organic contaminant absorption-desorption in recent years.
In essence, absorption is a dynamic process, and the dynamic approach and the technology that are used to study it are rapidly developed in recent decades, and become one of focus of research.It is not only the basis of understanding many courses of reaction, and is the main means that characterize the long-pending and pore structure of solid particles surface.Inquire into reaction mechanism by it, carry out reaction kinetics research and more and more be subject to people's attention.These dynamic methods need not vacuum system and dead volume measure, equipment is simple, generally design and installation voluntarily are easy to operate, easily repeat.How to study fast, convenient, dynamic flexibly absorption-desorption analytical approach, and it is significant aspect environmental protection successfully to apply to inquire into absorption and the mechanism of degradation of organism in the mineral matter micropore.
The utility model content
It is a kind of multiple functional that the purpose of this utility model is to provide, Gas Phase Adsorption-desorption apparatus that automaticity is high, not only can be as required sample introduction by different way, and can be to the online detection of absorption-desorption product, carry out qualitative, quantitative test.Easy and simple to handle, save cost.The gas chromatography detector that adopts in this device is applicable to organism, and is highly sensitive, is mainly used in absorption and the mechanism of degradation research of volatility halogenated hydrocarbons in the mineral matter micropore.Can suitably reequip it, the absorption-desorption dynamics that is applied to other materials is probed into.
For realizing above purpose, the utility model has been taked following technical scheme: a kind of Gas Phase Adsorption-desorption apparatus that possesses the auto injection analytic function, comprise the carrier gas supply system that connects successively, the dehydration and deoxidation pipe, the electron mass flowmeter, the organic steam generator, steam generator, sampling valve, first gas passage of sampling valve is connected to adsorption column, the adsorption column other end is connected to the gas circuit cross-over valve, the gas circuit cross-over valve comprises manual two-position valve and eight electronic valves, and from the first passage and the second channel of two-position valve output, two-position valve is connected the endpiece of adsorption column, two gas circuit cross-over valve can be realized continuous detecting and the conversion that intermittently detects, eight valves are connected the end of sampling valve gas circuit, being used for gas collects, described first passage connects back second gas passage of sampling valve, and second channel is connected to gas chromatography detector; Add a cold-trap at described organic steam generator, adsorption column places baking oven.
The organic steam generator places cold-trap, can regulate the concentration of organic steam in helium by the temperature of control cold-trap, avoids steam in follow-up ducted condensation.Described gas circuit cross-over valve is a two-position valve, and wherein two passages are linked to each other with gas chromatography detector with sampling valve respectively, can realize intermittently detecting the conversion with continuous detecting.
Preferably, in described carrier gas supply system, adopt the very little inert gas helium of relative atomic mass, and accurately control the flow velocity of carrier gas, the stainless-steel tube that the conveyance conduit employing of carrier gas is difficult for being corroded by the electron mass flowmeter as carrier gas.
Preferably, described organic steam generator places cold-trap, can regulate the concentration of organic steam in helium by the temperature that changes cold-trap, as long as temperature is certain, organic concentration is definite value just before the absorption, simultaneously, the temperature of the steam of generation is lower than room temperature, thereby has avoided steam in follow-up ducted condensation.
Preferably, described adsorption column by the glass dropper of two brachymemmas through assembling, load into a small amount of glass fiber and adsorbate in the glass dropper respectively after, the heat-shrinkable tube that is polytetrafluoroethylmaterial material by one section two sides couples together two sections glass droppers.Be connected with glass capillary column with the heat-shrinkable tube of PTFE/FEP material respectively at the every other two ends of glass dropper, with heating gun baking PTFE/FEP heat-shrinkable tube, the heat-shrinkable tube thawing of being heated, the port of cooling back dropper just and capillary column tightly combine, and do not have dead volume.
Preferably, at the gas circuit cross-over valve of one two of described adsorption column outlet terminations,, can manually control because this valve only need be changed once in each experimentation.Two passages are wherein linked to each other with gas chromatography detector with sampling valve respectively, can realize the conversion of intermittently detection and continuous detecting.When absorption-desorption speed is slow, can pass through the sampling valve sample introduction, the chromatographic column of flowing through is carried out the detection at intermittence, when absorption-desorption speed is very fast when maybe needing to obtain continuous data point, gas directly can be fed detecting device, carries out continuous detecting.
Preferably, connecing one at described gas circuit end can programme controlled eight gas circuit cross-over valve, connects resin column or other gas collectors at each endpiece of valve, and the material that the different time sections desorb is got off collects and carries out other analyses.
Preferably, described sampling valve is a ten-way valve that has two sample introduction positions, and this valve is a pneumatic valve, comes programmed control by gas chromatograph, and two onesize gasometry rings are installed on the valve, and when adopting the valve injection pattern, the every switch of valve once advances sample twice.Be about to before the absorption and the gas after the absorption takes turns sample introduction, can observe the variation of gas concentration more intuitively.
Preferably, described gas chromatograph can separate the different compounds that desorb, and is next qualitative according to retention time, can tentatively infer the reaction mechanism of adsorbate and adsorbate by the variation of classes of compounds.
The variation that described gas chromatograph adopts FID in parallel and ECD detecting device to detect organic concentration.Wherein FID has highly sensitively, and dead volume is little, and response is fast, and the range of linearity is wide, and advantages such as good stability are widely used in organic mensuration.And ECD is the detecting device of a kind of high sensitivity and high selectivity, and through being commonly used to analyze the component with electronegative element of trace, but its range of linearity is narrower.The two all has good response to volatility halogenated hydrocarbons and catabolite thereof.The two is combined, quantitative when concentration is higher with FID, come quantitatively can obtain best quantitative data with ECD when concentration is very low.
Preferably, described adsorbed gas circulation pipeline all adopts glass capillary, and glass or polytetrafluoroethylmaterial material are all adopted in the junction, have reduced absorption and have reached and the chemical reaction that installs.
A kind of absorption-desorption device that possesses the auto injection analytic function of the present utility model, obtain certain density low temperature organic steam by the control temperature, organic steam is taken in carrier gas out of, the steam generator of flowing through, enter into adsorption column and carry out adsorption reaction, realize continuous detecting and the conversion that intermittently detects with a two-position valve, and before will adsorbing with ten-way valve, after gas take turns sample introduction.FID and ECD parallel connection are detected.Connecing one at the end of gas circuit can be used for gas by programme controlled eight gas circuit cross-over valves and collect.
The utility model compared with prior art, have following advantage: the utility model is simple to operate, and is convenient, time saving and energy saving, can both obtain good experimental result to slow desorb and fast desorb, favorable reproducibility, the result is accurate and visual.Can well carry out qualitatively, quantitative test is a strong instrument of inquiring into the absorption degradation mechanism of volatile organic matter in the mineral micropore.
Description of drawings
Fig. 1 is a kind of structural representation that possesses the Gas Phase Adsorption-desorption apparatus of auto injection analytic function of the present utility model;
Fig. 2 is the structural representation to adsorption column among Fig. 1.
Embodiment
Below in conjunction with the drawings and specific embodiments content of the present utility model is described in further details.
Embodiment one:
As depicted in figs. 1 and 2, comprise the carrier gas supply system 1 that connects successively, dehydration and deoxidation pipe 2, electron mass flowmeter 3, organic steam generator 4, steam generator 5, sampling valve 6, first gas passage of sampling valve 6 is connected to adsorption column 7, adsorption column 7 other ends are connected to gas circuit cross-over valve 8, gas circuit cross-over valve 8 comprises manual two-position valve and eight electronic valves, and from the first passage 81 and the second channel 82 of two-position valve 8 output, two-position valve is connected the endpiece of adsorption column 7, eight valves are connected the end of sampling valve gas circuit, first passage 81 connects back second gas passage of sampling valve 6, and second channel 82 is connected to gas chromatography detector; Add a cold-trap at organic steam generator 4, adsorption column 7 places baking oven.
Helium is accurately controlled its flow by electron mass flowmeter 3 behind dehydration and deoxidation pipe 2, this section pipeline adopts stainless-steel tube, and follow-up pipeline all adopts glass capillary.Mass flowmeter 3 is linked to each other with organic steam generator 4, an end capillaceous inserts organic solution inside, add a cold-trap in organic steam generator 4 outsides, controlling its temperature is lower than more than room temperature 10 degree, so just can obtain certain density low temperature organic steam, avoid gas in follow-up ducted condensation, can regulate the concentration of organic steam in helium by the temperature that changes cold-trap simultaneously.Organic steam generator 4 is linked to each other with water vapor generator 5, and kapillary is inserted into below the water surface, and the water vapor generator is placed water-bath.Through just obtaining by steam-laden organic steam behind the water vapor generator.This gas enters into adsorption column 7 through sampling valve 6 and reacts.Adsorption column 7 is by the glass dropper 71 of two brachymemmas, 72 through assembling, at glass dropper 71, load a small amount of glass fiber 73 and adsorbate in 72 respectively, the heat-shrinkable tube 74 that is polytetrafluoroethylmaterial material with one section two sides couples together them then, two ends are connected with capillary column 76 with the heat-shrinkable tube 75 of double-deck PTFE/FEP material respectively in addition, with heating gun baking PTFE/FEP heat-shrinkable tube 75, make its fusing, cooling back glass dropper 71,72 port just tightly combines with kapillary 76, and does not have dead volume.Adsorption column 7 is placed baking oven, can utilize temperature programme to carry out thermal desorption.The gas that comes out from adsorption column 7 enters into one two gas circuit cross-over valve 8, first passage 81 connects back sampling valve 6 second valves, and second channel 82 is connected to gas chromatography detector, when intermittently detecting, gas enters into sampling valve 6 by first passage 81, and the chromatographic column of flowing through 91 is carried out separation detection.During continuous detecting, gas circuit cross-over valve 8 is switched to 81, gas directly enters into gas chromatography detector, obtains continuous data point.Gas circuit cross-over valve 8 is a hand valve, only needs conversion once in the experimentation.Sampling valve 6 is a ten-way valve that has two sample introduction positions, and this valve is a pneumatic valve, is controlled by gas chromatograph, and two onesize gasometry rings 61 and 62. are housed on the valve, the pilot-gas flow velocity is certain, and 2 μ L can be installed respectively, 5 μ L, 10 μ L, 15 μ L, 20 μ L, 25 μ L, 50 μ L, 100 μ L, 250 μ L, 500 μ L, 1mL, 2mL, 5mL, the quantitative ring of 10mL changes the quantitative ring of selecting best size according to the signal of detecting device.When adopting the valve injection pattern, the every switch of valve once (promptly switches once), advances sample twice, be about to absorption before, after gas take turns sample introduction.Gas chromatograph 9 adopts fid detector 92 in parallel and ECD detecting device 93 detection signal simultaneously, carries out qualitative and quantitative analysis.Connecing one at the end (being the outlet of sampling valve) of gas circuit can programme controlled eight gas circuit cross-over valve 10, connects fat attached column or other gas collectors at each endpiece of valve, and the material that the different time sections desorb is got off collects and carries out other analyses.
Embodiment 1 is applicable to the absorption-desorption experiment under the water environment, when the absorption-desorption under carrying out water-less environment is tested, steam generator 5 can be removed.
Embodiment two:
Present embodiment is basic identical with embodiment 1, does not just need water vapor generator 5, but organic steam generator 4 is directly linked to each other with sampling valve 6.
Above-listed detailed description is at the specifying of the utility model possible embodiments, and this embodiment is not in order to limiting claim of the present utility model, does not allly break away from the equivalence that the utility model does and implements or change, all should be contained in the claim of this case.
Claims (7)
1. Gas Phase Adsorption-desorption apparatus that possesses the auto injection analytic function, it is characterized in that: comprise the carrier gas supply system (1) that connects successively, dehydration and deoxidation pipe (2), electron mass flowmeter (3), organic steam generator (4), sampling valve (6), first gas passage of sampling valve (6) is connected to adsorption column (7), adsorption column (7) other end is connected to the gas circuit cross-over valve, the gas circuit cross-over valve comprises manual two-position valve (8) and electronic eight valves (10), and from the first passage (81) and the second channel (82) of two-position valve (8) output, two-position valve (8) is connected the endpiece of adsorption column (7), eight valves (10) are connected the end of sampling valve (6) gas circuit, described first passage (81) connects back second gas passage of sampling valve (6), and second channel (82) is connected to gas chromatography detector; Add a cold-trap at described organic steam generator (4), adsorption column (7) places baking oven.
2. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1, it is characterized in that: described adsorption column by the glass dropper of two brachymemmas through assembling, in the glass dropper, be filled with quantitative glass fiber and adsorbate respectively, and the heat-shrinkable tube that is polytetrafluoroethylmaterial material by one section two sides couples together two sections glass droppers; Be connected with glass capillary column with the heat-shrinkable tube of PTFE/FEP material respectively at the every other two ends of glass dropper.
3. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1 is at each endpiece connection resin column or gas collector of eight valves (10).
4. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1 is characterized in that: described sampling valve is a ten-way valve that has two sample introduction positions, and two onesize gasometry rings are installed on the valve.
5. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1 is characterized in that: described gas chromatograph adopts FID and ECD detecting device in parallel.
6. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1, it is characterized in that: the latter linked adsorbed gas circulation pipeline of described electron mass flowmeter (3) all adopts glass capillary, and glass or polytetrafluoroethylmaterial material are all adopted in the junction.
7. Gas Phase Adsorption-the desorption apparatus that possesses the auto injection analytic function according to claim 1 is characterized in that: also be connected with water vapor generator (5) between described organic steam generator (4) and sampling valve (6).
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| CN2011200619456U CN202033333U (en) | 2011-03-10 | 2011-03-10 | Gas-phase adsorption-desorption device having function of automatically analyzing injected samples |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102661992A (en) * | 2012-05-14 | 2012-09-12 | 华瑞科学仪器(上海)有限公司 | Ammonia gas concentration detection system and detection method thereof |
| CN104792604A (en) * | 2015-04-28 | 2015-07-22 | 李勘 | Electronic refrigeration atmosphere pre-concentrator |
| CN104990827A (en) * | 2015-06-15 | 2015-10-21 | 北京科技大学 | Determining method and device for adsorption quantity of low-volatility organic gas on adsorbing materials |
| CN105749583A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | General preparative two-dimensional liquid chromatography device and operation method thereof |
| CN106168548A (en) * | 2016-08-23 | 2016-11-30 | 中国科学院大气物理研究所 | Volatile material samples automatically/sampling device and method |
| CN106841483A (en) * | 2017-02-24 | 2017-06-13 | 苏州天蓝分析仪器有限公司 | A kind of sample introduction separator of ping-pong structure |
| CN108459122A (en) * | 2018-05-21 | 2018-08-28 | 泰通科技（广州）有限公司 | A kind of secondary parsing thermal desorption device of binary channels |
| CN110095541A (en) * | 2019-05-06 | 2019-08-06 | 南京工业大学 | A kind of gas separation characterization apparatus and mixed gas separating property detection method |
| CN110612440A (en) * | 2017-05-11 | 2019-12-24 | 松下电器产业株式会社 | Gas analysis method and gas analysis device |
| CN110646549A (en) * | 2019-11-06 | 2020-01-03 | 四川晟实科技有限公司 | Thermal desorption instrument and analysis system for volatile organic compound detection and working method thereof |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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2011
- 2011-03-10 CN CN2011200619456U patent/CN202033333U/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102661992B (en) * | 2012-05-14 | 2014-01-22 | 华瑞科学仪器(上海)有限公司 | Ammonia gas concentration detection system and detection method thereof |
| CN102661992A (en) * | 2012-05-14 | 2012-09-12 | 华瑞科学仪器(上海)有限公司 | Ammonia gas concentration detection system and detection method thereof |
| CN105749583B (en) * | 2014-12-16 | 2017-10-20 | 中国科学院大连化学物理研究所 | A kind of general preparative two-dimensional liquid chromatography device and its operating method |
| CN105749583A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | General preparative two-dimensional liquid chromatography device and operation method thereof |
| CN104792604A (en) * | 2015-04-28 | 2015-07-22 | 李勘 | Electronic refrigeration atmosphere pre-concentrator |
| CN104990827B (en) * | 2015-06-15 | 2019-02-01 | 北京科技大学 | The measuring method and equipment of low volatility organic gas adsorbance on the adsorbent material |
| CN104990827A (en) * | 2015-06-15 | 2015-10-21 | 北京科技大学 | Determining method and device for adsorption quantity of low-volatility organic gas on adsorbing materials |
| CN106168548A (en) * | 2016-08-23 | 2016-11-30 | 中国科学院大气物理研究所 | Volatile material samples automatically/sampling device and method |
| CN106841483A (en) * | 2017-02-24 | 2017-06-13 | 苏州天蓝分析仪器有限公司 | A kind of sample introduction separator of ping-pong structure |
| CN110612440A (en) * | 2017-05-11 | 2019-12-24 | 松下电器产业株式会社 | Gas analysis method and gas analysis device |
| CN108459122A (en) * | 2018-05-21 | 2018-08-28 | 泰通科技（广州）有限公司 | A kind of secondary parsing thermal desorption device of binary channels |
| CN110095541A (en) * | 2019-05-06 | 2019-08-06 | 南京工业大学 | A kind of gas separation characterization apparatus and mixed gas separating property detection method |
| CN110646549A (en) * | 2019-11-06 | 2020-01-03 | 四川晟实科技有限公司 | Thermal desorption instrument and analysis system for volatile organic compound detection and working method thereof |
| CN110646549B (en) * | 2019-11-06 | 2023-04-07 | 四川晟实科技有限公司 | Thermal desorption instrument and analysis system for volatile organic compound detection and working method thereof |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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Granted publication date: 20111109 Termination date: 20140310 |