CN101672833A - Device for enriching and desorbing gaseous sample - Google Patents

Device for enriching and desorbing gaseous sample Download PDF

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Publication number
CN101672833A
CN101672833A CN200910091410A CN200910091410A CN101672833A CN 101672833 A CN101672833 A CN 101672833A CN 200910091410 A CN200910091410 A CN 200910091410A CN 200910091410 A CN200910091410 A CN 200910091410A CN 101672833 A CN101672833 A CN 101672833A
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China
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heating furnace
sampling pipe
refrigeration piece
conductor refrigeration
gaseous sample
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CN200910091410A
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CN101672833B (en
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丁辉
赵寿堂
朱佐刚
胡玢
靳江红
王栋
朱小锋
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Beijing Municipal Institute of Labour Protection
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Beijing Municipal Institute of Labour Protection
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Abstract

The invention discloses a device for enriching and desorbing a gaseous sample, comprising a heating furnace, a semiconductor cooling block, sampling tubes and adsorbent filled inside the sampling tubes, wherein one end of the heating furnace is connected with the semiconductor cooling block; the heating furnace and the semiconductor cooling block are arranged on a lead rail in a sliding way; the outer end of the heating furnace or the semiconductor cooling block is connected with a power device which is used for pushing and pulling the heating furnace and the semiconductor cooling block to doreciprocating motion on the lead rail; a channel is respectively arranged inside the heating furnace and the semiconductor cooling block, and the two channels are penetrated and communicated with eachother; and the sampling tubes are arranged inside the channels formed by the heating furnace and the semiconductor cooling block. The device for enriching and desorbing the gaseous sample adopts thelow temperature sampling technique so as to improve the collection efficiency of the sample, leads enrichment and desorption of the sample to be sequentially completed within a short time, increases the analysis efficiency, reduces the analysis cost, and has the advantages of low power consumption, light weight, compact structure and being especially suitable for the application of portable gas chromatogram.

Description

Gaseous sample enrichment, desorption apparatus
Technical field
The present invention relates to a kind of gaseous sample enrichment, desorption apparatus, relate in particular to a kind of example enrichment, desorption apparatus that is applied to portable gas chromatograph.
Background technology
Though gas chromatograph is a kind of highly sensitive analytical instrument,, when the pollutant levels that will test during,, and can not carry out quantitative test because can not obtain enough signal responses less than the concentration limit of instrument.Under this test condition, will adopt sample enrichment, desorption technology to finish analysis.
Concentration enriching pollutants in the gaseous sample, desorption technology are a kind of sample-pretreating methods commonly used.At first select suitable sampling pipe according to the physical parameter of pollutant, the corresponding adsorbent of filling in the sampling pipe, adsorbent commonly used has: Tenax, acticarbon, Carbotrap etc. are used to adsorb gaseous contaminant of different nature.Enriching pollutants in the sample in sampling pipe after, add thermal desorption, finish the analysis of sample.Sample enrichment, desorption technology can be carried out concentrating of hundred times to sample, and the application of gas chromatograph has been expanded in the sensitivity that has improved gas chromatograph greatly.
At present, the device volume that is used for example enrichment, desorption is huge, and area heated is bigger, and therefore, power consumption is also bigger, is unsuitable for the use of portable gas chromatograph, does not especially use the cold trap trapping technology, and the sample concentration multiple is not high, and sampling efficiency is very low.
Summary of the invention
The purpose of this invention is to provide and a kind ofly in enrichment process, use the cold trap trapping technology, and cooling of switch sampling pipe and heated condition easily, compact conformation, the sampling efficiency height is suitable for gaseous sample enrichment, desorption apparatus that portable gas chromatograph is used.
In order to achieve the above object, a kind of gaseous sample enrichment provided by the present invention, desorption apparatus, it comprises: heating furnace, conductor refrigeration piece and sampling pipe and the adsorbent of wherein filling, end at described heating furnace is connected with the conductor refrigeration piece, in described heating furnace and described conductor refrigeration piece, respectively be provided with a passage, these two passages run through connection, and described sampling pipe places in it; Described heating furnace and conductor refrigeration piece are slidably disposed on the guide rail, perhaps, described sampling pipe is arranged on the guide rail, outer end at described heating furnace or conductor refrigeration piece, perhaps on described sampling pipe, connect a pulling device, be used for described heating furnace of push-and-pull and conductor refrigeration piece or the described sampling pipe of push-and-pull, make and move back and forth relative of described heating furnace and conductor refrigeration piece place the described passage of described conductor refrigeration piece thereby make sampling pipe alternately place the described passage of described heating furnace to neutralize with described sampling pipe.
This guide rail can be to be fixed on the basis.
The described pulling device that connects in the outer end of described heating furnace or conductor refrigeration piece is preferably propulsion system, moves back and forth with described heating furnace of push-and-pull and conductor refrigeration piece.
Described propulsion system can be to comprise air cylinder device, solenoid valve and gas storage steel cylinder, in the cylinder in this air cylinder device piston mandril is set, this piston mandril and described heating furnace or conductor refrigeration piece or sampling pipe are connected, be positioned on the described cylinder of these piston rod both sides air inlet/outlet is set, one described solenoid valve respectively is set on it, and this solenoid valve connects described gas storage steel cylinder by the gas circuit associated line.
Be connected by the gas circuit associated line between described cylinder and the described solenoid valve, also can be connected between this solenoid valve and this gas storage steel cylinder by the gas circuit associated line.
Solenoid valve is used for the action of control cylinder, and the gas storage steel cylinder provides the power of cylinder action.
The available metal rod is connected between described heating furnace and the described conductor refrigeration piece.
The bore of described sampling pipe can be 0.5mm-6mm, preferred 0.5-2mm.The length of this sampling pipe can be 3cm-10cm, and it can be a stainless-steel tube.Be provided with import and export on sampling pipe, connecting line on this is imported and exported is provided with corresponding valve on this pipeline.Make pollutant in the atmosphere enter and overflow this sampling pipe by this pipeline.
Described guide rail can be to be provided with like this: the corresponding cross through hole of described passage that the two bottom sides of described heating furnace is respectively equipped with and which is provided with, the corresponding through hole of described passage that the two bottom sides of described conductor refrigeration piece is respectively equipped with and which is provided with, heating furnace is corresponding with the described through hole that the conductor refrigeration piece is provided with, be interspersed with guide rail at this through hole, make described heating furnace and conductor refrigeration piece on guide rail, to be free to slide, to finish the relative motion between sampling pipe and heating furnace and the conductor refrigeration piece.
The two ends of described guide rail are respectively equipped with the prevention bolt, prevent the derailing of heating furnace and conductor refrigeration piece.
Described conductor refrigeration piece is two flaky semiconductor frigorific units, and it interconnects, and is provided with the gap in the middle of these two flaky semiconductor frigorific units and constitutes described passage, and this gap is greater than the diameter of sampling pipe; Heating furnace is a tubular heater, and caliber constitutes described passage greater than the sampling pipe external diameter.
Gaseous sample enrichment provided by the invention, desorption apparatus are by being provided with the conductor refrigeration piece, and provide special construction to make sampling pipe to change at the heating space and the cooling space of heating furnace and conductor refrigeration piece easily, make enrichment, adsorption process better to carry out, therefore, this device has following advantage:
1. gaseous sample enrichment of the present invention, desorption apparatus have adopted the low temperature Sampling techniques, have improved sample collecting efficient.
2. gaseous sample enrichment of the present invention, desorption apparatus have been realized the purpose that example enrichment, desorption convert successively at short notice, have improved analysis efficiency, have reduced analysis cost.
3. gaseous sample enrichment of the present invention, desorption apparatus provide a kind of sampling pipe of minor diameter small size, make its heating, cooling velocity improve, power consumption reduces, also make sample size reduce, can reduce like this to resolve and use gas, reach high concentration, the minimum of lowering apparatus detects concentration, improve the sensitivity of instrument, also make the peak broadening diminish, improved quantitative accuracy and separation efficiency;
4. the compact conformation of gaseous sample enrichment provided by the invention, desorption apparatus, in light weight, be particularly suitable for the application of portable gas chromatography.
Description of drawings
Fig. 1 is the structural representation of gaseous sample enrichment of the present invention, desorption apparatus.
Fig. 2 is the heating furnace shown in Figure 1 and the plan structure synoptic diagram of conductor refrigeration piece formation passage.
Fig. 3 is the structural representation that sampling pipe shown in Figure 1 moves into heating furnace.
Fig. 4 is sampling pipe shown in Figure 3 moves into heating furnace in passage a plan structure synoptic diagram.
Fig. 5 is the structural representation that sampling pipe shown in Figure 1 moves into the conductor refrigeration piece.
Fig. 6 is sampling pipe shown in Figure 5 moves into the conductor refrigeration piece in passage a plan structure synoptic diagram.
Number in the figure explanation: 1: propulsion system, 11: air cylinder device, 111: cylinder, 112: piston mandril, 12: gas circuit associated line, 13: solenoid valve, 14: gas storage steel cylinder, 2: conductor refrigeration piece, 21: the conductor refrigeration unit, 22: gap, 3: sampling pipe, 4: heating furnace, 5: metal bar, 6: guide rail, 7: stop bolt, 8: passage.
Embodiment
Extremely shown in Figure 6 as Fig. 1, a kind of gaseous sample enrichment of the present invention, desorption apparatus, this device comprises heating furnace 4, conductor refrigeration piece 2 and sampling pipe 3, fill adsorbent when in sampling pipe 3, using, heating furnace 4 is used for sampling pipe 3 heating, the adsorbent pollutant of desorption, adsorbent is Tenax, acticarbon, Carbotrap etc., end at described heating furnace 4 is connected with conductor refrigeration piece 2, its other end connects propulsion system 1, conductor refrigeration piece 2 is used for the cooling when the sampling pipe absorb polluted matter, helps the enrichment of pollutant, improves sample collecting efficient.In heating furnace 4 and conductor refrigeration piece 2, respectively be provided with a passage 8, these two passages run through connection, described sampling pipe 3 can move or leave standstill in the passage 8 of described heating furnace 4 and 2 formation of described conductor refrigeration piece, described conductor refrigeration piece 2 and described heating furnace 4 are under the push-and-pull action of propulsion system 1, move back and forth, thereby during sampling pipe 3 and place in the conductor refrigeration piece 2 formed part passages, the time and place in the heating furnace 4 formed part passages.
Described propulsion system 1 comprise air cylinder device 11, solenoid valve 13, gas storage steel cylinder 14, connect gas circuit associated line 12 on the air inlet/outlet on the cylinder 111 of air cylinder device 11, be connected with gas storage steel cylinder 14 by associated line 12, on this associated line 12, solenoid valve 13 be set.Piston mandril 112 in the air cylinder device 11 is connected with the body of heater of heating furnace 4, the piston mandril 112 of air cylinder device 11 also can be fixed on the outside housing of conductor refrigeration piece 2, air cylinder device 11 is fixed on the appropriate location in the apparatus structure, so that its swimmingly the heating furnace and the conductor refrigeration piece that connect together of push-and-pull move back and forth, make sampling pipe or in heating furnace 13, or in conductor refrigeration piece 2.Solenoid valve 13 is used for the action of control piston push rod 112, and gas storage steel cylinder 14 provides the power of air cylinder device 11 actions.
Be connected with metal bar 5 between described heating furnace 4 and the described conductor refrigeration piece 2.
The bore of described sampling pipe 3 is stainless-steel tubes of 0.5mm-6mm, and its length can be at 3cm-10cm.
Described heating furnace 4 and conductor refrigeration piece 2 are slidably disposed on the guide rail 6, the integrated structure of this guide rail and heating furnace and conductor refrigeration piece can be: the two bottom sides of described heating furnace 4 is respectively equipped with and described passage 8 corresponding cross through hole, the two bottom sides of described conductor refrigeration piece 2 is respectively equipped with and described passage 8 corresponding through holes, two described through holes are corresponding, corresponding through hole is interspersed with guide rail 6, heating furnace 4 and conductor refrigeration piece 2 can be free to slide on two guide rails 6, two track symmetric arrangement, heating furnace and conductor refrigeration piece are operated steadily, and guide rail 6 is fixed on the appropriate location in the apparatus structure.
The two ends of described guide rail 6 are respectively equipped with and stop bolt 7, prevent heating furnace 4 and 2 derailings of conductor refrigeration piece.
Described conductor refrigeration piece 2 is two flaky semiconductor frigorific units 21, and middle gap 22 becomes described passage 8 greater than the diameter of sampling pipe 3; Heating furnace 4 is tubular heaters, and its caliber becomes described passage 8 greater than sampling pipe 3 external diameters.
During use, extremely shown in Figure 6 as Fig. 1, when carrying out sample collecting, switch by solenoid valve 13, cylinder 111 left cylinder cavities inflation in air cylinder device 11 outer, the piston mandril 112 of air cylinder device 11 moves to right-hand, pulling conductor refrigeration piece 2 and heating furnace 4 also move to right-hand on guide rail 6, stop to move until the gap 21 that sampling pipe 3 is arranged in conductor refrigeration piece 2 this moment, conductor refrigeration piece 2 beginning refrigeration are simultaneously opened the sampling gas circuit that is connected with the import of sampling pipe simultaneously and are carried out sample collecting.After sample collecting is finished, close the sampling gas circuit, switch by solenoid valve 13, the cylinder 111 right cylinder cavities inflation of air cylinder device 11, the piston mandril 112 of air cylinder device 11 moves to left, promoting conductor refrigeration piece 2 and heating furnace 4 moves to left on guide rail 6, be positioned at heating furnace 4 until sampling pipe 3 and stop to move this moment, and heating furnace 4 begins heating simultaneously, waits to reach the sample desorption temperature, open the sample analysis gas circuit that is connected with the outlet of sampling pipe, carry out sample analysis.Being respectively equipped with one at the two ends of guide rail 6 stops bolt 7 to prevent conductor refrigeration piece 2 and heating furnace 4 derailings.The present invention has realized the enrichment process of sample cold trap trapping of portable instrument and the desorption process of heating by said structure, and makes that the conversion of heating process and cooling procedure is convenient and swift.In the present embodiment, sampling pipe 3 selects specification to be: internal diameter 0.5mm, external diameter 0.75mm, length 3cm, wherein the sampling pipe adsorbent of filling Tenax.
The conductor refrigeration piece of the bore of above-mentioned sampling pipe and smaller power and heating furnace cooperate can be in very short and time accurately heating or be cooled to absorption or the needed temperature of desorption.For example, the power of conductor refrigeration piece 2 is 40W, can make the temperature of sampling pipe 3 drop to-20 ℃ from room temperature in 5 seconds, has improved the sampling efficiency of 3 pairs of benzene series things of sampling pipe, halogenated hydrocarbons and ester class, alcohols etc. greatly.Heating furnace 4 power are 20W, can make the temperature of sampling pipe 3 be raised to 250 ℃ from room temperature in 10 seconds, have improved the desorption efficiency of sample.In specific implementation process, can select the power of conductor refrigeration piece and heating furnace according to parameters such as the fill-up of adsorbent in the sampling pipe and the selections of sampling pipe material.In case selected, be applied in the concrete instrument, can carry out temperature survey to sampling pipe, simplify apparatus structure.

Claims (10)

1. gaseous sample enrichment, desorption apparatus, it is characterized in that: it comprises: heating furnace, conductor refrigeration piece and sampling pipe and the adsorbent of wherein filling, end at described heating furnace is connected with the conductor refrigeration piece, in described heating furnace and described conductor refrigeration piece, respectively be provided with a passage, these two passages run through connection, described sampling pipe places in it, described heating furnace and conductor refrigeration piece are slidably disposed on the guide rail, perhaps, described sampling pipe is arranged on the guide rail movably, connect a pulling device in the outer end of described heating furnace or conductor refrigeration piece or on described sampling pipe, with the described heating furnace of push-and-pull and conductor refrigeration piece or the described sampling pipe of push-and-pull, make and move back and forth relative of described heating furnace and conductor refrigeration piece place the described passage of described conductor refrigeration piece thereby make sampling pipe alternately place the described passage of described heating furnace to neutralize with described sampling pipe.
2. a kind of gaseous sample enrichment according to claim 1, desorption apparatus, it is characterized in that: described pulling device is propulsion system, it comprises air cylinder device, solenoid valve and gas storage steel cylinder, piston mandril in this air cylinder device is arranged in the cylinder, be positioned on the described cylinder of these piston mandril both sides air inlet/outlet is set, one described solenoid valve respectively is set on it, be connected by the gas circuit associated line between described solenoid valve and described gas storage steel cylinder, described piston mandril and described heating furnace or described conductor refrigeration piece or sampling pipe are connected.
3. a kind of gaseous sample enrichment according to claim 1 and 2, desorption apparatus is characterized in that: be connected by metal bar between described heating furnace and the described conductor refrigeration piece.
4. according to the described a kind of gaseous sample enrichment of one of claim 1 to 3, desorption apparatus, it is characterized in that: the caliber of described sampling pipe is the stainless-steel tube of 0.5mm-6mm; And/or the length of described sampling pipe is 3-10cm.
5. a kind of gaseous sample enrichment according to claim 4, desorption apparatus is characterized in that: the internal diameter 0.5mm of described sampling pipe, external diameter 0.75mm, length 3cm.
6. a kind of gaseous sample enrichment according to claim 1, desorption apparatus, it is characterized in that: the two bottom sides of described heating furnace is respectively equipped with two cross through hole, the two bottom sides of described conductor refrigeration piece is respectively equipped with cross through hole, the described through hole of described heating furnace and conductor refrigeration piece is corresponding, and corresponding through hole is interspersed with described guide rail.
7. according to claim 1 or 6 described a kind of gaseous sample enrichments, desorption apparatus, it is characterized in that: the two ends of described guide rail are respectively equipped with the prevention bolt.
8. a kind of gaseous sample enrichment according to claim 1, desorption apparatus is characterized in that: described conductor refrigeration piece is two flaky semiconductor frigorific units, and the gap in the middle of it is greater than the external diameter of described sampling pipe; And/or described heating furnace is a tubular heater, and its bore is greater than described sampling pipe external diameter.
9. according to the described a kind of gaseous sample enrichment of one of claim 1 to 8, desorption apparatus, it is characterized in that: the coupling of the power of described conductor refrigeration piece and the caliber of described sampling pipe made the temperature that is in the described sampling pipe in the described conductor refrigeration piece drop to-20 ℃ from room temperature in 5 seconds; And/or,
The coupling of the power of described heating furnace and the caliber of described sampling pipe made the temperature that is in the described sampling pipe in the described heating furnace be raised to 250 ℃ from room temperature in 10 seconds.
10. according to the described a kind of gaseous sample enrichment of one of claim 1 to 9, desorption apparatus, it is characterized in that: described sampling pipe is a stainless-steel tube; And/or wherein the adsorbent of Tian Chonging is Tenax or acticarbon or Carbotrap.
CN2009100914100A 2009-08-20 2009-08-20 Device for enriching and desorbing gaseous sample Expired - Fee Related CN101672833B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
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CN102128896A (en) * 2010-11-19 2011-07-20 聚光科技(杭州)股份有限公司 Sampling method and device
CN102735523A (en) * 2011-03-29 2012-10-17 国家海洋局第一海洋研究所 Automatic translation and lifting type trapping and desorbing device and manufacturing method of same
CN103852370A (en) * 2014-03-04 2014-06-11 天津市环境保护科学研究院 Mobile low-temperature adsorption concentration-thermal desorption device and application method thereof
CN104458974A (en) * 2014-11-19 2015-03-25 华南理工大学 Pretreatment device and method for determining trace hydrogen phosphide employing gas chromatography method
CN104483423A (en) * 2014-12-31 2015-04-01 同方威视技术股份有限公司 Sample collection and thermal analysis sampling device and method as well as trace detection device
CN105319304A (en) * 2015-12-14 2016-02-10 河南省建筑科学研究院有限公司 Portable gas chromatograph used for detecting VOC (Volatile Organic Compounds) in indoor air
CN105928745A (en) * 2016-06-14 2016-09-07 马鞍山十七冶工程科技有限责任公司 Activated air sampling pipe fixture
CN109342581A (en) * 2018-09-26 2019-02-15 上海交通大学 A kind of adsorption system comprehensive performance analysing device and the analysis method based on the device
CN112179750A (en) * 2020-09-14 2021-01-05 聚光科技(杭州)股份有限公司 Enrichment apparatus and method

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CN2430687Y (en) * 2000-05-26 2001-05-16 中国石油化工集团公司 Adsorption concentrated desorption device
CN100353164C (en) * 2005-01-28 2007-12-05 北京大学 On-line analyzer for atmospheric volatile organic compounds
CN201133905Y (en) * 2007-12-28 2008-10-15 上海烟草(集团)公司 Column box outer cooling heater for single column box multidimensional gas chromatograph

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102128896A (en) * 2010-11-19 2011-07-20 聚光科技(杭州)股份有限公司 Sampling method and device
CN102735523A (en) * 2011-03-29 2012-10-17 国家海洋局第一海洋研究所 Automatic translation and lifting type trapping and desorbing device and manufacturing method of same
CN103852370A (en) * 2014-03-04 2014-06-11 天津市环境保护科学研究院 Mobile low-temperature adsorption concentration-thermal desorption device and application method thereof
CN104458974A (en) * 2014-11-19 2015-03-25 华南理工大学 Pretreatment device and method for determining trace hydrogen phosphide employing gas chromatography method
CN104483423A (en) * 2014-12-31 2015-04-01 同方威视技术股份有限公司 Sample collection and thermal analysis sampling device and method as well as trace detection device
EP3242130A4 (en) * 2014-12-31 2018-09-05 Nuctech Company Limited Sample collection, thermal analysis, and sample injection apparatus and method, and trace detection device
US10215666B2 (en) 2014-12-31 2019-02-26 Nuctech Company Limited Sample injection device and method for sample collection and sample thermal desorption, and trace detection apparatus
CN105319304A (en) * 2015-12-14 2016-02-10 河南省建筑科学研究院有限公司 Portable gas chromatograph used for detecting VOC (Volatile Organic Compounds) in indoor air
CN105928745A (en) * 2016-06-14 2016-09-07 马鞍山十七冶工程科技有限责任公司 Activated air sampling pipe fixture
CN109342581A (en) * 2018-09-26 2019-02-15 上海交通大学 A kind of adsorption system comprehensive performance analysing device and the analysis method based on the device
CN112179750A (en) * 2020-09-14 2021-01-05 聚光科技(杭州)股份有限公司 Enrichment apparatus and method
CN112179750B (en) * 2020-09-14 2023-11-14 聚光科技(杭州)股份有限公司 Enrichment apparatus and method

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