CN112179750B - Enrichment apparatus and method - Google Patents
Enrichment apparatus and method Download PDFInfo
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- CN112179750B CN112179750B CN202010957525.XA CN202010957525A CN112179750B CN 112179750 B CN112179750 B CN 112179750B CN 202010957525 A CN202010957525 A CN 202010957525A CN 112179750 B CN112179750 B CN 112179750B
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 230000017525 heat dissipation Effects 0.000 claims abstract description 19
- 238000005057 refrigeration Methods 0.000 claims description 11
- 239000004065 semiconductor Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 description 18
- 238000003795 desorption Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Devices That Are Associated With Refrigeration Equipment (AREA)
Abstract
The invention provides an enrichment device and a method, wherein the enrichment device comprises an enrichment unit; the inside of the container is in a vacuum state; the enrichment unit is arranged in the container; the input end of the first pipeline is arranged outside the container, the output end of the first pipeline is communicated with the inlet of the enrichment unit, the output end of the second pipeline is arranged outside the container, and the input end of the second pipeline is communicated with the outlet of the enrichment unit; the refrigerator is provided with a hot end and a cold end, the hot end is arranged outside the container, and the cold end is arranged in the container; the first heat dissipation unit is arranged outside the container and is provided with a contact surface in the container; the second heat radiating unit is arranged at the hot end; a heater is arranged in the container and is used for heating the enrichment unit; the drive unit is used for driving the enrichment unit so that the enrichment unit selectively contacts the contact surface and the cold end. The invention has the advantages of high enrichment efficiency and the like.
Description
Technical Field
The present invention relates to gas detection, and in particular to enrichment apparatus and methods.
Background
Atmospheric VOCs, due to their low concentration, often need to be enriched and concentrated for the sample to be detected. Particularly, for some high-volatility low-carbon compounds, low-temperature enrichment and rapid temperature rise thermal desorption are often required.
The main stream technology in the current market is high-temperature desorption after adsorption by adopting enrichment filler, and the common flow is as follows: cooling the enrichment pipe, sampling, thermal desorption sampling, high-temperature back blowing of the enrichment pipe and cooling the enrichment pipe; the temperature rising rate during thermal desorption sample injection has important influence on chromatographic peak type and instrument sensitivity, and the faster the temperature rising is, the more concentrated the desorption is, the better the instrument peak type is, and the higher the sensitivity is; the cooling time of the enrichment tube has an important influence on the analysis period, and the analysis period can be shortened by reducing the cooling time, especially for a method with shorter separation time, the analysis period can be directly shortened by shortening the cooling time of the enrichment tube.
In order to solve the problems of time-sharing cooling and heating, the prior art gives a solution method that: heating and refrigeration are carried out in situ, specifically: placing the enrichment tube in a cold trap, and indirectly heating the enrichment tube by a heating wire or directly heating the enrichment tube by electrifying during desorption; after the desorption is finished, refrigerating through a cold trap, so that the enrichment tube is subjected to slow heat exchange and cooling; semiconductor refrigeration or thermo-acoustic refrigeration is generally used for refrigeration. The technical scheme has a plurality of defects, such as:
1. when the rich pipe is heated quickly, a large amount of heat can be directly transferred to the refrigerator, and the heat conduction structure on the surface of the refrigerator is easy to damage;
2. when heating, a large amount of heat is transferred to the refrigerator, so that the refrigerator is in overload operation, and the service life of the refrigerator is greatly reduced;
3. because the refrigeration temperature is between-150 ℃ and 40 ℃, the heat preservation difficulty is high, the freezing of the inside of the cold trap cavity is easy to cause, the cooling efficiency is affected, and the frequent maintenance is needed;
4. the detection efficiency is low, and when the desorption state is converted into the enrichment state, namely, the high-temperature refrigeration is carried out to the low temperature, the time consumption is long, and the overall detection efficiency is reduced.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the enrichment device with high detection efficiency, good reliability and long service life.
The invention aims at realizing the following technical scheme:
an enrichment device comprising an enrichment unit; the enrichment device further comprises:
a container, wherein the container is in a vacuum state; the enrichment unit is arranged in the container;
the input end of the first pipeline is arranged outside the container, the output end of the first pipeline is communicated with the inlet of the enrichment unit, the output end of the second pipeline is arranged outside the container, and the input end of the second pipeline is communicated with the outlet of the enrichment unit;
the refrigerator is provided with a hot end and a cold end, the hot end is arranged outside the container, and the cold end is arranged in the container;
the first heat dissipation unit is arranged outside the container and is provided with a contact surface in the container; the second heat radiating unit is arranged at the hot end;
a heater disposed within the container for heating the enrichment unit;
and the driving unit is used for driving the enrichment unit so that the enrichment unit selectively contacts the contact surface and the cold end.
The invention also aims to provide an enrichment method using the enrichment device, and the aim of the invention is achieved by the following technical scheme:
an enrichment method, wherein the enrichment method comprises the following steps:
under the action of a driving unit, an enrichment unit in the container contacts the cold end;
the temperature of the gas in the enrichment unit is reduced, and the components to be detected are enriched and remain in the enrichment unit;
under the action of the driving unit, the enrichment unit is separated from the cold end;
the heater works, and the components to be detected in the enrichment unit are released and sent to the downstream;
under the action of the driving unit, the enrichment unit contacts with the first heat dissipation unit, and the temperature in the enrichment unit is reduced;
in the above process, the inside of the container is in a vacuum state.
Compared with the prior art, the invention has the following beneficial effects:
in order to overcome the defects in the prior art, the applicant proposes a split design, namely, heating, cooling and refrigerating are performed separately, and introduces a technical idea of performing the heating, cooling and refrigerating in a vacuum state. Based on the inventive concept, the following steps are achieved:
1. the detection efficiency is high;
after thermal desorption is completed, the heater or the enrichment unit is driven by the precursor to adhere to the first heat dissipation unit, heat is conducted to the first heat dissipation unit, and then the heat is dissipated into the air outside the container, so that the temperature of the enrichment unit is rapidly reduced; then, the heater or the enrichment unit is driven to be abutted against the cold end of the refrigerator, so that the enrichment unit is rapidly cooled; the cooling of the first heat radiating unit is utilized, so that the load of the refrigerator is obviously reduced, the subsequent detection efficiency is improved, and the service life of the refrigerator is prolonged;
the heating and the refrigerating are carried out in a vacuum environment, so that the heating and the refrigerating have high efficiency, and the detection efficiency is further improved;
the cold end of the first heat radiating unit and/or the refrigerator is provided with a shape matched with the heater or the enrichment unit, such as a groove shape, so that the contact area is increased, and the heating efficiency and the refrigerating efficiency are correspondingly improved;
2. the reliability is good, and the service life is long;
the heating and the refrigerating are completed in different areas, so that the refrigerator is prevented from being damaged when the enrichment unit is heated rapidly, and the service life of the refrigerator is correspondingly prolonged;
the heat reflection layer is arranged so that when the heater or the enrichment unit contacts the first heat dissipation unit to cool down, heat of the heater or the enrichment unit is prevented from radiating to the refrigerator.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic diagram of an enrichment device according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these embodiments that fall within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1:
FIG. 1 schematically shows a schematic structural diagram of an enrichment device according to an embodiment of the present invention, as shown in FIG. 1, the enrichment device includes:
enrichment unit 31, such as a enrichment pipe; the enrichment unit 31 is a prior art in the field, and the specific structure and working principle are not described here again;
the container 11 is in a vacuum state, for example, the container is closed after being vacuumized, or the container is communicated with a pump, the pressure in the container is monitored, and the pump is started in real time, so that the vacuum in the container is maintained; the enrichment unit 31 is arranged in the container 11;
a first pipe 51 and a second pipe 52, wherein the input end of the first pipe 51 is arranged outside the container 11, and the output end of the first pipe is communicated with the inlet of the enrichment unit 31 and is used for sending gas into the enrichment unit 31; the output end of the second pipeline 52 is arranged outside the container 11, and the input end of the second pipeline is communicated with the outlet of the enrichment unit 31 and is used for discharging the gas which is not enriched in the enrichment unit 31;
a refrigerator, such as a semiconductor refrigerator or a thermo-acoustic refrigerator, having a hot end 62 and a cold end 61, the hot end 62 being disposed outside the vessel 11 and the cold end 61 being disposed within the vessel 11;
a first heat dissipating unit 21 and a second heat dissipating unit 22, such as a radiator with a fan, the first heat dissipating unit 21 being disposed outside the container and having a contact surface inside the container; the second heat dissipation unit 22 is arranged at the hot end;
a heater 41, such as an electric heater, the heater 41 being disposed within the container for heating the enrichment unit 31;
and the driving unit is driven by a cylinder or a motor and is used for driving the enrichment unit, so that the enrichment unit selectively contacts the contact surface and the cold end.
In order to improve the heating efficiency, further, the heater is arranged around the enrichment unit, such as the enrichment unit is arranged in the heater with the cylindrical structure.
In order to increase the contact area and improve the cooling or refrigerating efficiency, the shape of the contact surface and/or the cold end is matched with the outer wall of the heater or the enrichment unit, such as the contact surface is in a groove shape
In order to reduce the influence of the heat radiation of the heater or the enrichment unit on the refrigerator during heating or cooling, further, the cold end is provided with a heat reflecting layer.
The enrichment method of the embodiment of the invention, namely the working method of the enrichment device of the embodiment, is that:
under the action of a driving unit, an enrichment unit in the container contacts the cold end;
the temperature of the gas in the enrichment unit is reduced, and the components to be detected are enriched and remain in the enrichment unit;
under the action of the driving unit, the enrichment unit is separated from the cold end;
the heater works, and the components to be detected in the enrichment unit are released and sent to downstream analysis;
under the action of the driving unit, the enrichment unit contacts with the first heat dissipation unit, and the temperature in the enrichment unit is reduced;
in the above process, the inside of the container is in a vacuum state.
In order to prevent mutual influence, further, when the heater works, the enrichment unit is not contacted with the cold end and the first heat dissipation unit.
Example 2:
application example of the enrichment apparatus and method according to embodiment 1 of the present invention.
In the application example, the enrichment unit adopts an enrichment pipe, and the inside of the enrichment pipe is provided with a filler; the heater adopts an electric heating pipe with a cylindrical structure, and the enrichment pipe is arranged in the heater;
one end of the first pipeline is communicated with the inlet of the enrichment pipe, and the other end of the first pipeline extends out of the container and keeps sealing with the container wall; one end of the second pipeline is communicated with the outlet of the enrichment pipe, and the other end of the second pipeline extends out of the container and keeps sealing with the container wall; the first pipeline and the second pipeline are made of flexible materials;
the first radiating unit comprises a radiator and a radiating fan, the radiator is fixed on the first side wall of the container, part of the radiator is positioned in the container, the other part of the radiator is positioned outside the container, and the radiating fan is arranged outside the container; the part of the radiator in the container is provided with a groove matched with the outer wall of the heater;
the refrigerator adopts semiconductor refrigeration and is fixed on a second side wall (a first side wall and a second side wall are oppositely arranged) of the container, wherein a cold end is positioned in the container, a hot end is positioned outside the container, a heat reflection layer is arranged on the side surface of the cold end, which is opposite to the first heat dissipation unit, and the shape of the side surface is a groove matched with the outer wall of the heater; the second heat dissipation unit comprises a radiator and a heat dissipation fan, and is arranged on the hot end;
an air pump, wherein an inlet of the air pump is communicated with the inside of the container; the pressure sensor is arranged in the container, and when the monitored pressure is higher than a threshold value, the air pump is automatically started, so that the vacuum degree in the container is ensured;
the cylinder is disposed within the container for pushing the heater up and down such that the heater is selectively located in a heating position (contacting neither the cold end nor the first heat dissipating unit), a cooling position (i.e., contacting the heat sink of the first heat dissipating unit), and a cooling position (i.e., contacting the cold end).
The enrichment method of the embodiment of the invention, namely the working method of the enrichment device of the embodiment, is that:
under the action of the air cylinder, the heater contacts the cold end, the contact area of the groove-shaped contact surface is increased, and the refrigeration efficiency is improved;
the gas enters a enrichment pipe from a first pipeline, the temperature of the gas in the enrichment pipe is reduced, the components to be detected are enriched and remain in an enrichment unit, and other gas components are discharged through a second pipeline;
under the action of the air cylinder, the enrichment unit is separated from the cold end and is positioned at a heating position;
the heater works, and the components to be detected in the enrichment unit are released and sent to downstream analysis;
under the action of the air cylinder, the enrichment unit contacts with the first heat dissipation unit, and the temperature in the enrichment unit is reduced; the groove-shaped contact surface improves the contact area and the cooling efficiency;
in the above process, the vacuum state is maintained in the container.
Example 3:
an application example of the enrichment device and method according to embodiment 1 of the present invention is different from embodiment 2 in that:
the heater is of two semi-cylindrical structures and is combined into a cylinder; the two parts are combined into a cylinder shape or separated under the drive of a cylinder or a motor; the rich pipe is driven up and down by an air cylinder or a motor and is selectively positioned at a cooling position, a heating position and a refrigerating position according to the requirement; linear driving of the heater and enrichment tube is well known in the art.
The enrichment method of the embodiment of the invention, namely the working method of the enrichment device of the embodiment, is that:
under driving, the two semi-cylindrical parts of the heater are separated;
under the drive, the enrichment tube moves downwards to contact with the cold end, and the groove-shaped contact surface of the cold end matched with the cylindrical structure of the enrichment tube improves the contact area and the refrigeration efficiency;
the gas enters a enrichment pipe from a first pipeline, the temperature of the gas in the enrichment pipe is reduced, the components to be detected are enriched and remain in an enrichment unit, and other gas components are discharged through a second pipeline;
under the drive, the enrichment unit moves upwards to be separated from the cold end and is positioned at a heating position; the heater is driven to be combined into a cylinder shape, and the rich pipe is wrapped from the periphery;
the heater works, and the components to be detected in the enrichment unit are released and sent to downstream analysis;
under driving, the two semi-cylindrical parts of the heater are separated;
driven by the first heat dissipation unit, the enrichment pipe moves upwards to contact with the first heat dissipation unit, and the temperature in the enrichment unit is reduced; the groove-shaped contact surface of the radiator matched with the cylindrical structure of the enrichment pipe improves the contact area and the cooling efficiency;
in the above process, the vacuum state is maintained in the container.
The above embodiments only exemplify that the heater and the cold end adopt grooves matched with the cylindrical outer wall of the heater or the enrichment pipe, and of course, the heater may also have a quadrangular prism structure, and correspondingly, the shapes of the grooves of the radiator and the cold end of the first heat radiating unit are matched with the outer wall of the heater, so that the contact area is increased, and the efficiency of temperature change is further improved.
Claims (7)
1. According to the enrichment method of the enrichment device, the enrichment device comprises an enrichment unit, and is characterized in that the enrichment device further comprises;
a container, wherein the container is in a vacuum state; the enrichment unit is arranged in the container;
the input end of the first pipeline is arranged outside the container, the output end of the first pipeline is communicated with the inlet of the enrichment unit, the output end of the second pipeline is arranged outside the container, and the input end of the second pipeline is communicated with the outlet of the enrichment unit;
the first heat dissipation unit is arranged outside the container and is provided with a contact surface in the container; the first radiating unit comprises a radiator and a radiating fan, the radiator is fixed on the first side wall of the container, part of the radiator is positioned in the container, the other part of the radiator is positioned outside the container, and the radiating fan is arranged outside the container;
the refrigerator is fixed on the second side wall of the container and is provided with a hot end and a cold end, the hot end is positioned outside the container, and the cold end is positioned in the container; the first side wall and the second side wall are oppositely arranged;
the second heat dissipation unit is arranged at the hot end;
a heater disposed within the container for heating the enrichment unit; the heater is of two semi-cylindrical structures, and is combined into a cylindrical shape or separated under the driving of an air cylinder or a motor;
the driving unit is used for driving the enrichment unit so that the enrichment unit selectively contacts the contact surface and the cold end;
the enrichment method comprises the following steps:
under driving, the two semi-cylindrical parts of the heater are separated; under the action of a driving unit, an enrichment unit in the container contacts the cold end;
the temperature of the gas in the enrichment unit is reduced, and the components to be detected are enriched and remain in the enrichment unit;
under the action of the driving unit, the enrichment unit is separated from the cold end and is positioned at a heating position; the heater is driven to be combined into a cylinder shape, and the enrichment unit is wrapped from the periphery;
the heater works, and the components to be detected in the enrichment unit are released and sent to the downstream;
under the drive, the two semi-cylindrical parts of the heater are separated, and under the action of the drive unit, the enrichment unit contacts with the first heat dissipation unit, and the temperature in the enrichment unit is reduced;
in the process, the inside of the container is in a vacuum state;
when the heater works, the enrichment unit is not contacted with the cold end and the first heat dissipation unit.
2. The enrichment method according to claim 1, wherein: the shape of the contact surface and/or cold end is matched with the outer wall of the heater or enrichment unit.
3. The enrichment method according to claim 2, wherein: the contact surface is in a groove shape.
4. The enrichment method according to claim 1, wherein: the cold end has a heat reflective layer.
5. The enrichment method according to claim 1, wherein: the refrigerator is semiconductor refrigeration or thermo-acoustic refrigeration.
6. The enrichment method according to claim 1, wherein: the driving unit adopts an air cylinder.
7. The enrichment method according to claim 1, wherein the enrichment device further comprises:
and the input end of the pump is communicated with the interior of the container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010957525.XA CN112179750B (en) | 2020-09-14 | 2020-09-14 | Enrichment apparatus and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010957525.XA CN112179750B (en) | 2020-09-14 | 2020-09-14 | Enrichment apparatus and method |
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| CN112179750A CN112179750A (en) | 2021-01-05 |
| CN112179750B true CN112179750B (en) | 2023-11-14 |
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| CN202010957525.XA Active CN112179750B (en) | 2020-09-14 | 2020-09-14 | Enrichment apparatus and method |
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| CN114324719A (en) * | 2021-12-20 | 2022-04-12 | 杭州谱育科技发展有限公司 | Online detection method and device for peculiar smell in water body |
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| JPWO2011099079A1 (en) * | 2010-02-12 | 2013-06-13 | ジーエルサイエンス株式会社 | Sample collection method and collection device |
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| JPH08327615A (en) * | 1995-03-24 | 1996-12-13 | Shimadzu Corp | Sampler |
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