CN112577781A - Thermal analysis device for aerosol sampling of linear conversion adsorption sheet - Google Patents
Thermal analysis device for aerosol sampling of linear conversion adsorption sheet Download PDFInfo
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- CN112577781A CN112577781A CN202011458400.9A CN202011458400A CN112577781A CN 112577781 A CN112577781 A CN 112577781A CN 202011458400 A CN202011458400 A CN 202011458400A CN 112577781 A CN112577781 A CN 112577781A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/622—Ion mobility spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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Abstract
The invention provides an aerosol sampling thermal analysis device of a linear conversion adsorption sheet, which realizes synchronous sampling and analysis by switching the adsorption sheet in an aerosol sampling gas path switching and linear sliding mode, and provides a new thought for a rapid online efficient sampling, enrichment and analysis method of an aerosol sample. Meanwhile, the sampling air passage can be changed or arrayed according to the requirement to realize multi-point sampling analysis, and the whole device and the whole process are very suitable for automatic control.
Description
Technical Field
The invention relates to an aerosol sampling and thermal analysis device in the field of gas sampling, in particular to a device for thermal analysis after sampling aerosol particles, which is mainly applied to analysis instruments such as ion mobility spectrometry, mass spectrometry and the like.
Background
The technology about aerosol sampling has been many in the analytical instruments such as applied to ion mobility spectrometry, mass spectrometry, for example, patent CN102478466A adopts the impact aerosol sampling technology, after collecting a sample to a certain area of a long sampling belt, rotates the sampling belt, and sends the part of the sampling belt with the sample to a thermal analysis device, then carries out analysis. In patent CN201921473231.9, an impact aerosol sampling technique is also adopted, and after a sample is collected on a specific sampling sheet, the sampling sheet with the sample is sent to a thermal analysis device for analysis under the drive of a rotating shaft. A common feature of these patents is that aerosol samples are collected and then analyzed. Common for this is: 1. enriching a sample; 2. and collecting required samples, and eliminating interference of other samples. 3. Is suitable for on-line sampling analysis.
The invention is inspired by the above patents, realizes sample enrichment, interference elimination and online sampling analysis, and meanwhile, mainly innovates the flow mode of an aerosol sampling gas circuit, redesigns the mode of a long sampling belt or a rotating shaft for transmitting and collecting samples into a left-right linear sliding mode, namely completes sample enrichment collection and online analysis, and also can realize single-channel or multi-channel sample collection. Compared with the patent CN102478466A, the method has the advantages of simultaneous sampling and analysis, and for the patent CN201921473231.9, the method has the advantages of simultaneous sampling at multiple points, greatly prolonging the enrichment time, improving the sampling throughput and improving the analysis flux; the single-pass sampling can realize the automatic switching of sampling air flow, improve the sampling efficiency and realize the purpose of single-point sampling and multi-point analysis.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides an aerosol sampling thermal analysis device with a linear conversion adsorption sheet, mainly solves the problem of an aerosol sampling gas path flow mode, and realizes single-channel or multi-channel sample collection.
In order to achieve the purpose, the invention adopts the technical scheme that:
a linear conversion adsorption sheet aerosol sampling thermal analysis device comprises a sampling enrichment unit, a thermal analysis unit and a transmission unit; the transmission unit comprises a support frame, the sampling enrichment unit is fixed at two ends of the support frame, the thermal analysis unit is fixed in the middle of the support frame, and the transmission unit is fixed on the support frame;
the sampling enrichment unit comprises single-point sampling and multi-point sampling; the single-point sampling and the multi-point sampling both comprise sampling air passages and sampling ports;
the single-point sampling air passage is in an inverted Y shape, has a three-way structure and comprises a public air passage and two branch air passages communicated with the public air passage, and the outlets of the two branch air passages are sampling ports, wherein in the sampling process, the two branch air passages cannot be communicated with the public air passage simultaneously;
the multipoint sampling device comprises at least two mutually independent sampling air passages, wherein any one sampling air passage is in a straight shape and is vertical to a support frame, and the outlet of each sampling air passage is a sampling port;
the sampling ports of the single-point sampling and the multi-point sampling are both positioned above the two ends of the support frame.
The thermal analysis unit comprises a thermal analysis assembly and an analysis port; the thermal desorption assembly is used for gasifying the aerosol sample at high temperature, and the desorption port is used for placing the sample to be gasified;
the transmission unit comprises a linear slide rail, a slide block and at least one adsorption sheet; the linear slide rail is two parallel guide rails; the slider is arranged on the guide rail and can move along the guide rail, a through hole is formed in the middle of the slider, the through hole is matched with the sampling port and the analysis port in size, and the adsorption sheet covers the through hole.
Preferably, the linear slide rail is provided with a gear or a fixed transmission belt, so that the position conversion of the slide block at the sampling port and the position conversion of the slide block at the analysis port are realized, and the adsorption sheet is driven to convert the positions of the sampling port and the analysis port.
Preferably, the thermal analysis device further comprises a driving device I, and the driving device I is used for driving the sliding block to move linearly, so as to drive the adsorption sheet to realize the conversion between the sampling port and the analysis port.
Preferably, the absorbent sheet is an air permeable mesh.
Preferably, the sampling enrichment unit further comprises two airflow switching airway valves and an air extractor, wherein the two airflow switching airway valves are respectively positioned between the common airway and the two branch airways of the sampling airway and play a role in opening and closing the airways; the air exhaust device is respectively positioned below the two sampling ports and can move along the axial direction of the two branch air passages.
Preferably, the thermal resolution assembly is positioned above the middle position of the support frame and is in an inverted concave shape, and an air chamber is formed at the groove of the concave structure; an analytic opening is formed at the opening of the groove; the thermal desorption unit further comprises a desorption gas circuit, and the desorption gas circuit comprises a gas inlet pipe and a gas outlet pipe which are communicated with the gas chamber.
Preferably, the thermal analysis assembly further comprises a heating rod and a temperature sensor fitted to the gas chamber.
Preferably, the thermal analysis unit further comprises a sample injection head, and the sample injection head is located below the gas chamber and used for sealing the gas chamber.
Preferably, the thermal desorption unit further comprises a driving device II, wherein the driving device II is installed below the sample injection head and used for driving the sample injection head to move up and down, and the adsorption sheet is sealed between the gas chamber of the thermal desorption assembly and the sample injection head.
The invention also provides an aerosol analysis system, which combines the linear conversion adsorption sheet aerosol sampling thermal analysis device with ion mobility spectrometry or mass spectrometry.
The transmission unit comprises a linear slide rail, a slide block, an adsorption sheet and a driving device I. The linear slide rail is a pair of parallel guide rails, the slide block is fixed on the linear slide rail, the drive device I utilizes a gear or a transmission belt to realize the linear slide of the slide block on the linear slide rail, the central through hole of the slide block is covered with the adsorption sheet, and the through hole on the drive device I is controlled to be respectively adapted to the sampling port and the analysis port, so that the adsorption and analysis of a sample are realized. The adsorption sheet is of a net structure, so that ventilation is facilitated.
The material of the adsorption sheet is a high-temperature-resistant fabric or paper material, and more preferably a high-temperature-resistant mesh fabric; the high temperature resistance means the temperature resistance of 200-250 ℃.
The thermal analysis unit is used for gasifying the collected aerosol sample at high temperature and sending the gas into the detection unit, and comprises a thermal analysis assembly, a support piece and a driving device II (preferably an axial displacement driving device). One end of the thermal resolution component is provided with a groove to form an air chamber. The support is interposed between the driving means II and the thermal desorption assembly. The driving device II can be a stepping motor or an electromagnetic valve and the like.
The linear slide preferably has a pair of parallel rails or a single-sided rail.
The sampling air passage can be in a Y shape or two straight-line shapes and other forms, if the sampling air passage is in the Y shape, 1-point sampling can be realized, and different analysis methods are adopted; and the multipoint sampling analysis can be realized if the character is a straight character.
The adsorption sheet is made of an adsorption material. The adsorption piece and the sliding block can be fixedly sealed by adopting methods such as gluing or clamping.
In order to meet the requirements of the existing aerosol sampling and sample introduction on high sensitivity, rapid sampling analysis, combined application of a plurality of analysis methods and the like, the invention also combines the principle of an impact collector and a thermal analysis analyzer, is characterized in that an innovation is made on the aerosol sampling gas path flow mode, and designs a linear conversion adsorption sheet aerosol sampling thermal analysis device, so that the online rapid acquisition of the aerosol is realized, and the acquired sample is sent into an ion mobility spectrometry or a mass spectrometry through the thermal analysis analyzer for rapid analysis. Meanwhile, multipoint sample collection or multi-path sample analysis can be realized by changing the gas path flow and expanding the collection and enrichment unit or the thermal analysis unit. The sampling injector can increase sampling time, improve enrichment sensitivity and improve the utilization rate of analysis and detection especially in the array sampling channel.
The invention has the advantages that:
(1) under the condition of strict requirements on sampling and analysis timeliness, synchronous sampling and analysis can be realized, the sampling enrichment unit also starts sampling when a sample is analyzed, and the analysis time is fully utilized. The analysis time is shorter than the sampling time under general conditions, and the sampling uninterrupted process is realized by the Y-shaped air flow switching air passage switching mode, so that quasi-continuous sampling is really realized, and the requirement of high throughput analysis is met.
(2) The multi-point sampling or multi-path sampling analysis function can be conveniently realized by changing the air passage.
Drawings
The invention is described in further detail below with reference to the accompanying drawings:
FIG. 1 is a schematic structural diagram of a single sampling point linear conversion adsorption sheet aerosol sampling thermal desorption device.
Fig. 2 is a schematic structural diagram of an aerosol sampling thermal analysis device with two sampling points linearly switched adsorption sheets.
In the figure, 1, 28 samples the airway; 2. 13 an absorbent sheet; 3. 12, a sliding block; 4, a linear slide rail; 5, supporting a frame; 6. 11, 20 through holes; 7. 19 an air extraction device; 8. 18 a drive device I; 9 a sample introduction head; 10 driving device II; 14 thermal desorption assembly; 15 air chamber; 16 air outlet pipes; 17 air inlet pipes; 21. 22 valve stop bolts; 23. 26 a valve shaft; 24. 27 airflow switching airway valve; 25 a sample inlet; 29. 30 sampling ports; 31 a first sampling airway; 32 a second sampling airway; 33 analysis port.
Detailed Description
The invention provides a thermal analysis device for sampling aerosol of a linear conversion adsorption sheet, which is further described in detail according to a specific embodiment. In the present embodiment, unless otherwise specified, terms of orientation such as "upper", "lower", "left" and "right" used herein are defined with reference to the drawing plane of the corresponding drawing.
Fig. 1 is a schematic structural view of a single-point linear conversion adsorption sheet aerosol sampling thermal analysis device, which comprises a sampling enrichment unit, a thermal analysis unit and a transmission unit, wherein the sampling enrichment unit is fixed at two ends of a support frame 5, the thermal analysis unit is fixed in the middle of the support frame 5, the transmission unit is fixed on the support frame 5, and through holes 6, 11 and 20 are respectively arranged at the alignment positions of the sampling enrichment unit, the thermal analysis unit and the transmission unit.
The sampling and enriching unit is used for collecting, adsorbing and enriching an aerosol sample to be detected, the single-point sampling unit is divided into a left sampling and enriching unit and a right sampling and enriching unit, the left side comprises a sampling air passage 1, a sampling port 29 and an air exhaust device 7, and the right side comprises a sampling air passage 28, a sampling port 30 and an air exhaust device 19.
The whole air flow switching air passage is preferably of a Y-shaped large-caliber cylindrical structure and is in a tee joint shape. The inlet of the public air passage is an aerosol sample inlet 25, the two branch air passages are left and right sampling air passages 1 and 28, the outlet of the air passage is a left and right sampling port 29 and 30, and the branch positions of the air passages are provided with a left and right air flow switching air passage valves 24 and 27 respectively for realizing air passage switching.
The other side of the sampling ports 29, 30 opposite to the sampling gas channels 1, 28 is provided with a gas extraction device 7, 19, preferably any large flow enabling gas flow device, such as a gas pump or a fan. The air suction devices 7 and 19 can move along the axial directions of the sampling air passages 1 and 28, so that the air passages of the sampling enrichment units are sealed, and the adsorption sheets 2 and 13 on the sliding blocks 3 and 12 can be sealed between the air suction devices and the sampling air passages.
The thermal analysis unit is used for gasifying the collected aerosol sample at high temperature and sending the gas into an external analysis instrument, and comprises a thermal analysis component 14, an analysis port, an analysis gas path and a driving device II 10. One end of the thermal analysis component 14 is provided with a groove to form an air chamber 15, the air chamber 15 is communicated with the analysis port, the support frame 5 is positioned between the driving device II 10 and the analysis port, and the sample injection head 9 can move up and down under the driving of the driving device II 10, so that the air chamber 15 can be sealed. The thermal desorption gas circuit is provided with a gas inlet pipe 17 and a gas outlet pipe 16. The inlet pipe 17 extends vertically through the thermal analysis assembly 14 and is in communication with the gas chamber 15, and an outlet pipe 16 extends through the thermal analysis assembly 14 on the horizontal side of the thermal analysis assembly 14 and is also in communication with the gas chamber 15.
The transmission unit comprises a linear slide rail 4, sliders 3 and 12, adsorption pieces 2 and 13 and driving devices I8 and 18 (motors), and the driving devices I8 and 18 can realize the linear reciprocating motion of the sliders 3 and 12 on the linear slide rail 4. The adsorption pieces 2 and 13 are covered on the sliding blocks 3 and 12 to realize linear reciprocating transmission. The adsorption piece is at least one piece, when the adsorption piece is two pieces, the transmission unit is used for transmitting the adsorption piece which is enriched with the aerosol sample to the analysis port of the thermal analysis unit from the sampling port of the sampling and enrichment unit on one side, and the other adsorption piece which is not enriched with the aerosol sample can be transmitted back to the sampling port of the sampling and enrichment unit on the other side from the analysis port of the thermal analysis unit.
The linear slide rail 4 is preferably a pair of parallel guide rails fixed on the support frame 5, the sliding blocks 3 and 12 are placed on the guide rails, the driving devices I8 and 18 are preferably positioned between the sampling enrichment unit and the thermal analysis unit and also fixed on the support frame 5, and the sliding blocks 3 and 12 are linearly switched between the sampling enrichment unit and the thermal analysis unit through gears and a transmission belt. During sampling and analysis, the centers of the sliding blocks 3 and 12 are provided with through holes which correspond to the through holes 6, 11 and 20 on the supporting frame 5 and are used for gas circulation and up-and-down movement of the sampling head. The absorbent sheets 2, 13 are typically circular absorbent webs. The suction sheets 2, 13 are glued or clamped to the slide.
The working process of the whole device is illustrated by taking two adsorption sheets at a single sampling point as an example:
the working mode of the sampling enrichment unit is as follows: under the action of the driving device I8, the slide block 3 moves linearly along the linear guide rail to the sampling port 29 between the sampling air channel 1 and the air suction device 7, and the adsorption piece 2 without a sample covers the slide block 3 and therefore moves to the sampling port 29. Similarly, the adsorption sheet 13 is moved to the analysis opening. The adsorption piece 2, the through hole 6 and the sampling port 29 are coaxial, and the air extractor 7 moves upwards to seal the sliding block 3 and the adsorption piece 2 between the sampling air channel 1 and the air extractor 7 to form a closed air channel. At this time, the air extractor 7 is started to form negative pressure in the sampling air passage 1, the air flow switching air passage valve 24 is driven by the air flow to rotate along the valve rotating shaft 23 to be opened, and the air flow switching air passage valve 27 is closed by the blocking of the valve blocking bolt 22 due to the air pressure. At the moment, the left sampling air passage 1 is opened, the right sampling air passage 28 is closed, and the aerosol sample is driven by the air flow to impact the adsorption sheet 2 along the left sampling air passage 1, so that the aerosol sample is adsorbed, enriched and collected. And after the collection is carried out for a certain time, the sampling enrichment process is finished, and the sampling is finished.
If the right sampling air passage 28 is used for sampling, the air extractor 1 is started, negative pressure is formed in the sampling air passage 28, the air flow switching air passage valve 27 is driven by air flow to rotate along the valve rotating shaft 26 to be opened, and the air flow switching air passage valve 24 is closed by the blocking of the valve blocking bolt 21 due to air pressure. At this time, the right sampling airway 28 is open and the left sampling airway 1 is closed.
The working process of the thermal analysis unit is as follows: under the action of the driving device I8, the slide block 3 moves linearly along the linear guide rail to the analysis port between the thermal analysis assembly 14 and the sample injection head 9, and the adsorption sheet 2 with the sample covers the slide block 3, so the adsorption sheet moves to the analysis port. Similarly, the suction pad 13 is moved to the sampling port 30. The adsorption sheet 2, the thermal desorption assembly 14 and the through hole 11 are coaxial; the driving device II 10 moves the sample introduction head 9 upwards, the adsorption sheet 2 is sealed on the air chamber 15, the sample is heated, the carrier gas flow flows through the air inlet pipe 17 and reaches the air chamber 15, the gasified sample is taken out from the air outlet pipe 16 and sent into an analysis instrument, such as an ion mobility spectrometry or a mass spectrum. After a certain time of analysis, the sample injection analysis process is finished, and the analysis sample injection is completed.
The whole working process of the sample injector is as follows: firstly, collecting aerosol samples of the left sampling unit on the adsorption sheet 2, sending the adsorption sheet 2 to a thermal analysis unit by the transmission unit after sampling is completed, analyzing the samples, and sending the adsorption sheet 13 which is not analyzed last time and has no samples to the right sampling unit for sampling. The two sampling channels are alternately performed, and the sampling and analyzing processes can be performed synchronously. The time is saved, and the sampling analysis process is accelerated.
As shown in fig. 2, if multi-point sampling is to be implemented, the gas flow switching airway is set as a separate sampling and enrichment unit, and the sampling and enrichment units are arrayed, and each sampling and enrichment unit may be set with an independent transmission unit, so as to implement multi-point independent sampling and analysis, for example, the first sampling airway 31 and the second sampling airway 32 are installed with the thermal analysis unit 14 in between, which is common to both, so as to implement different point sample collection and analysis.
The working process is as follows: assuming that the first sampling air channel 31 starts sampling at this moment, the thermal analysis unit 14 is analyzing the sample in the second sampling air channel 32, and after a certain time, the sampling and analyzing processes are both finished, the transmission unit moves the adsorption sheet of the second sampling air channel 32 out of the thermal analysis unit 14, and sends the adsorption sheet of the first sampling air channel 31 into the thermal analysis unit 14 to start analysis, and the second sampling air channel 32 starts sampling at the same time. After a certain time, the sampling and analyzing process is finished, and the above process is repeated and circulated continuously, so that the sampling analysis of different sampling points is realized.
Claims (10)
1. The aerosol sampling thermal analysis device is characterized by comprising a sampling enrichment unit, a thermal analysis unit and a transmission unit; the transmission unit comprises a support frame, the sampling enrichment unit is fixed at two ends of the support frame, the thermal analysis unit is fixed in the middle of the support frame, and the transmission unit is fixed on the support frame;
the sampling enrichment unit comprises single-point sampling and multi-point sampling; the single-point sampling and the multi-point sampling both comprise sampling air passages and sampling ports;
the single-point sampling air passage is in an inverted Y shape, has a three-way structure and comprises a public air passage and two branch air passages communicated with the public air passage, and the outlets of the two branch air passages are sampling ports, wherein in the sampling process, the two branch air passages cannot be communicated with the public air passage simultaneously;
the multipoint sampling device comprises at least two mutually independent sampling air passages, wherein any one of the sampling air passages is in a straight shape and is vertical to the direction of a support frame, and the outlet of the sampling air passage is a sampling port;
the thermal analysis unit comprises a thermal analysis assembly and an analysis port; the thermal desorption assembly is used for gasifying the aerosol sample at high temperature, and the desorption port is used for placing the sample to be gasified;
the transmission unit comprises a linear slide rail, a slide block and at least one adsorption sheet; the linear slide rail is two parallel guide rails; the slider is arranged on the guide rail and can move along the guide rail, a through hole is formed in the middle of the slider, the through hole is matched with the sampling port and the analysis port in size, and the adsorption sheet covers the through hole.
2. The aerosol sampling thermal analysis device according to claim 1, wherein the linear slide rail is provided with a gear or a fixed transmission belt, so that the position conversion of the slide block at the sampling port and the analysis port is realized, and the position conversion of the adsorption sheet at the sampling port and the analysis port is driven.
3. The aerosol sampling thermal analysis device according to claim 1, wherein the thermal analysis device further comprises a driving device I, and the driving device I is used for driving the sliding block to move linearly so as to drive the adsorption sheet to realize the switching between the sampling port and the analysis port.
4. The aerosol sampling thermal analysis apparatus of claim 1, wherein the absorbent sheet is an air permeable mesh.
5. The aerosol sampling thermal analysis device according to claim 1, wherein the sampling enrichment unit further comprises two air flow switching air passage valves and an air pumping device, and the two air flow switching air passage valves are respectively positioned between the common air passage and the two branch air passages of the sampling air passage and play a role of opening and closing the air passages; the air exhaust device is respectively positioned below the two sampling ports and can move along the axial direction of the two branch air passages.
6. The aerosol sampling thermal desorption device of claim 1 wherein the thermal desorption assembly is positioned above the middle position of the support frame and is in an inverted concave shape, and an air chamber is formed at the groove of the concave structure; an analytic opening is formed at the opening of the groove; the thermal desorption unit further comprises a desorption gas circuit, and the desorption gas circuit comprises a gas inlet pipe and a gas outlet pipe which are communicated with the gas chamber.
7. The aerosol sampling thermal analysis apparatus of claim 1, wherein the thermal resolution assembly further comprises a heater rod and a temperature sensor fitted to the gas chamber.
8. The aerosol sampling thermal desorption device of claim 6 wherein the thermal desorption unit further comprises a sample injection head positioned below the gas chamber for sealing the gas chamber.
9. The aerosol sampling thermal analysis device according to claim 8, wherein the thermal analysis unit further comprises a driving device II, and the driving device II is installed below the sample injection head and used for driving the sample injection head to move up and down, so that the adsorption sheet is sealed between the gas chamber of the thermal analysis assembly and the sample injection head.
10. An aerosol analysis system comprising the aerosol sampling thermal desorption device of any one of claims 1 to 9 in combination with ion mobility spectrometry and mass spectrometry.
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| CN202011458400.9A CN112577781A (en) | 2020-12-10 | 2020-12-10 | Thermal analysis device for aerosol sampling of linear conversion adsorption sheet |
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| CN102455318A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院大连化学物理研究所 | Continuous monitor for detecting aerosol sample |
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Application publication date: 20210330 |