CN209841796U - A water trap and sampling device for concentrated sampling of gas - Google Patents
A water trap and sampling device for concentrated sampling of gas Download PDFInfo
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- CN209841796U CN209841796U CN201822034507.5U CN201822034507U CN209841796U CN 209841796 U CN209841796 U CN 209841796U CN 201822034507 U CN201822034507 U CN 201822034507U CN 209841796 U CN209841796 U CN 209841796U
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Abstract
The utility model discloses a water trap and sampling device for concentrated sampling of gas, this water trap: the method comprises the steps of removing water from sample gas through a first cold trap pipe filled with hydrophilic materials, concentrating the sample gas through a concentrated cold trap pipe, conveying organic matters and moisture desorbed by the first cold trap pipe in a pyrogenic state to a second cold trap pipe which is in a refrigerating state and filled with hydrophobic organic matter adsorption materials through carrier gas, adsorbing the organic matters desorbed by the first cold trap pipe, taking the moisture desorbed by the first cold trap pipe out of the second cold trap pipe through the carrier gas, conveying the organic matters desorbed by the first cold trap pipe and the second cold trap pipe in the pyrogenic state to the concentrated cold trap pipe through the carrier gas, and concentrating. Therefore, the utility model discloses can reduce concentrated sampling in-process, with losing of the higher component of the close component of water polarity and boiling point, improve the rate of recovery.
Description
Technical Field
The utility model relates to a gas chromatograph pretreatment technical field, in particular to a water trap and sampling device for gas concentration sampling.
Background
For detecting volatile and semi-volatile organic compounds, a gas chromatograph or a gas chromatograph-mass spectrometer is generally adopted, and as the organic compounds with very low detection content are difficult to meet the requirements by adopting a direct detection method and the detector sensitivity of the instrument, enrichment and concentration are required, and then the enriched and concentrated samples are eluted to obtain high-concentration samples for analysis, particularly for the volatile organic compounds in the air. The thermal desorption is a green sample injection mode which adopts a heating mode and elutes the components to be detected concentrated in the adsorbent into the gas chromatograph through inert gas, and the thermal desorption is more and more widely applied. However, each link in the whole process influences the analysis result.
The gas sampling mode of thermal desorption is generally divided into three types, namely sample tube sampling, tank sampling and on-line sampling, and the traditional thermal desorption on-line sampling generally introduces sample gas into a sample concentration cold trap tube through a vacuum pump for concentration and then desorbs the sample gas so as to obtain a lower detection limit. For an air sample, no matter which sampling mode is adopted, the component contains moisture, moisture entering the instrument can affect the instrument, cause great deviation on the qualitative and quantitative properties of the component, and even damage the instrument, so that water removal is one of the necessary functions of the thermal desorption instrument.
The water removal mode of thermal desorption online sampling mainly comprises two modes of organic membrane water removal and low-temperature water removal. The organic membrane dehydration is realized by leading polar molecules (moisture) introduced into the organic membrane tube to pass through the membrane and reach an external dry low-pressure gas environment, and non-polar molecules enter the concentration cold trap tube through a pipeline; the low-temperature water removal is realized by adopting a special material pipe or a pipe with a water absorbing material, when the sample gas passes through the pipe, water is intercepted, and most of the components to be detected enter the concentrated cold trap pipe through the water removal pipe. However, both of these water removal methods result in partial loss of some components, resulting in low recovery. For example, organic film removal can result in partial loss of polar components similar to water polarity, and conventional low temperature removal can result in heavy components (such as ozone precursors ethylene, ethane to dodecane, etc., which are more likely to remain in the water removal pipe with higher boiling points) remaining in the water removal pipe, resulting in low recovery.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a: the water removal device and the sample introduction device for gas concentration sampling can reduce loss of components with similar water polarity and components with higher boiling points in the concentration sampling process.
In order to realize the purpose of the utility model, the utility model provides a following technical scheme:
the utility model also provides a water removal device for gas concentration sampling, which comprises a first cold trap, a second cold trap, a concentration cold trap and a control module; wherein the content of the first and second substances,
hydrophilic materials are filled in the cold trap pipe of the first cold trap;
the cold trap pipe of the second cold trap is filled with hydrophobic organic matter adsorption material;
three connection relations are included; wherein the content of the first and second substances,
the first connection relation: the control module is connected with the first cold trap, the concentration cold trap and a controllable valve on a pipeline, the first cold trap is connected with the concentration cold trap, and the control module is used for enabling sample gas of a sample gas source to sequentially pass through cold trap pipes of the first cold trap and the concentration cold trap; wherein the first cold trap and the concentration cold trap are both operated in a refrigerated state;
the second connection relation: the control module is connected with the first cold trap, the second cold trap and a controllable valve on a pipeline and is used for enabling carrier gas of a carrier gas source to sequentially pass through cold trap pipes of the first cold trap and the second cold trap; wherein the first cold trap works in a heating state, and the second cold trap works in a cooling state;
the third connection relationship is: the control module is connected with the first cold trap, the second cold trap and a controllable valve on a pipeline, and the first cold trap, the second cold trap and the concentrated cold trap are sequentially connected and used for enabling carrier gas of a carrier gas source to respectively pass through cold trap pipes of the first cold trap and the second cold trap and then enter the cold trap pipe of the concentrated cold trap; wherein the first cold trap and the second cold trap work in a heating state.
According to a specific embodiment, the present invention is used in a water removal device for gas concentration sampling, wherein the first cold trap, the second cold trap and the concentration cold trap are all provided with a heating component, a cooling component and a temperature sensing element; and the control module controls the power of the heating component or the cooling component according to the temperature data detected by the temperature sensing elements of the first cold trap, the second cold trap and the concentration cold trap.
According to a specific embodiment, the utility model discloses a water trap for concentrated sampling of gas still includes pressure regulator for adjust the pressure of the carrier gas that the carrier gas source lets in.
The utility model also provides a sample feeding device for gas concentration sampling, which is based on the water removing device for gas concentration sampling, and also comprises a fourth connection relation; wherein, the fourth connection relation is as follows: the control module is connected with the concentration cold trap and a controllable valve on a pipeline and is used for leading carrier gas of a carrier gas source to enter a cold trap pipe of the concentration cold trap so as to convey organic matters desorbed from the cold trap pipe of the concentration cold trap to an analysis instrument or a sampling pipe; wherein the concentration cold trap works in a desorption state; thereby realizing the concentration and sampling of the gas and the automatic control of the sample introduction of the analyzer.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model is used for water trap of gas concentration sampling, first cold trap pipe through the packing has hydrophilic material to the dewatering of sample gas, rethread concentration cold trap pipe is concentrated sample gas, after that the organic matter and the moisture that will first cold trap pipe dissolve the suction under the pyrogenicity state are carried to being in the refrigeration state and are filled the second cold trap pipe that has hydrophobic organic matter adsorbing material through the carrier gas, and the organic matter that dissolves the suction to first cold trap pipe adsorbs, and the moisture that will first cold trap pipe dissolve the suction through the carrier gas takes out the second cold trap pipe, then carry the organic matter that first cold trap pipe and second cold trap pipe dissolve the suction under the pyrogenicity state to concentration cold trap pipe through the carrier gas, concentrate. Therefore, the utility model discloses can reduce concentrated sampling in-process, with losing of the higher component of the close component of water polarity and boiling point, improve the rate of recovery.
Description of the drawings:
fig. 1 is a schematic structural diagram of a water removal device for gas concentration sampling according to the present invention;
fig. 2 is a schematic view of the utility model used for a sampling device for gas concentration sampling.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. However, it should not be understood that the scope of the above-mentioned subject matter is limited to the following embodiments, and all the technologies realized based on the present invention are within the scope of the present invention.
The utility model provides a dewatering method for concentrated sampling of gas, it includes following step:
a: and introducing the sample gas into a first cold trap pipe which is in a refrigerating state and filled with hydrophilic materials for dewatering, and introducing the sample gas passing through the first cold trap pipe into a concentration cold trap pipe which is in the refrigerating state for concentration. Specifically, the hydrophilic material filled in the first cold trap pipe is especially selected from a hydrophilic material with weak organic matter adsorption capacity, such as glass wool.
b: and introducing carrier gas into the first cold trap pipe in a heating state, conveying the components desorbed from the first cold trap pipe to a second cold trap pipe in a refrigerating state and filled with hydrophobic organic matter adsorbing materials through the carrier gas, adsorbing the organic matters desorbed from the first cold trap pipe, and taking the water desorbed from the first cold trap pipe out of the second cold trap pipe through the carrier gas. Specifically, the hydrophobic organic matter adsorption material filled in the second cold trap pipe is Tenax.
c: and introducing carrier gas into the first cold trap pipe and the second cold trap pipe which are in a heating state at the same time, and conveying the organic matters desorbed from the first cold trap pipe and the second cold trap pipe to the concentration cold trap pipe in a refrigerating state by the carrier gas for concentration. Wherein the material filled in the concentrating cold trap tube is related to the component to be concentrated, and the skilled person can select the material according to specific requirements.
Furthermore, in the water removal method for gas concentration sampling of the present invention, the temperature of the refrigeration state of the first cold trap pipe and the second cold trap pipe is-10 to-50 ℃, and the heating state is 100-.
In addition, after the water removal is completed by adopting the water removal method for gas concentration sampling in the sample introduction process, the concentrated components in the concentrated cold trap pipe are desorbed, namely the concentrated cold trap pipe is heated to the desorption temperature, the carrier gas is introduced into the concentrated cold trap pipe, and the organic matters desorbed from the concentrated cold trap pipe are conveyed to an analysis instrument or a sampling pipe by the carrier gas. Wherein, the temperature of the concentration cold trap pipe in the desorption state is related to the property of the organic matters concentrated by the concentration cold trap pipe.
As shown in fig. 1, the water removal device for gas concentration sampling of the present invention includes a first cold trap 1, a second cold trap 2, a concentration cold trap 3 and a control module. Wherein, the first cold trap pipe 100 is filled with hydrophilic material; the second cold trap pipe 200 is filled with a hydrophobic organic substance adsorbing material. The concentrated cold trap 3 has a concentrated cold trap tube 300.
The control module comprises three control modes; wherein the content of the first and second substances,
the first control mode: the first cold trap 1 and the concentration cold trap 3 are controlled to work in a refrigerating state, and controllable valves are arranged on pipelines, so that sample gas of the sample gas source sequentially passes through the first cold trap pipe 100 and the concentration cold trap pipe 300, and the sample gas is sequentially subjected to dehydration and concentration.
The second control mode: and controlling the first cold trap 1 to work in a heating state, the second cold trap 2 to work in a cooling state, and controlling a controllable valve on a pipeline to enable carrier gas of a carrier gas source to sequentially pass through the first cold trap pipe 100 and the second cold trap pipe 200, wherein a hydrophobic organic matter adsorption material is filled in the second cold trap pipe 200 to adsorb organic matters desorbed from the first cold trap pipe 100, and meanwhile, the carrier gas takes water desorbed from the first cold trap pipe 100 out of the second cold trap pipe 200.
A third control mode: controlling the first cold trap 1 and the second cold trap 2 to work in a heating state, controlling the concentration cold trap 3 to work in a cooling state, and controlling the controllable valves on the pipelines to enable carrier gas of the carrier gas source to respectively pass through the first cold trap pipe 100 and the second cold trap pipe 200 and then enter the concentration cold trap pipe 300, so that organic matters desorbed from the first cold trap pipe 100 and the second cold trap pipe 200 are concentrated.
Specifically, the first cold trap 1, the second cold trap 2, and the concentrated cold trap 3 are each provided with a heating part, a cooling part, and a temperature sensing element. And the control module controls the power of the heating component or the cooling component according to the temperature data detected by the temperature sensing elements of the first cold trap, the second cold trap and the concentration cold trap. In practice, a pressure regulator may be provided in the input line of the carrier gas source for regulating the pressure of the carrier gas introduced by the carrier gas source, and the pressure regulator may be controlled by the control module.
The utility model is used for among the dewatering device of the concentrated sampling of gas, specific pipeline structure can be connected through a certain amount of pipelines and controllable valve and constitute, moreover, the field of technical personnel can be according to the gas passage relation that corresponds under each control mode of control module, confirm pipeline structure respectively with first cold trap pipe, the second cold trap pipe, concentrated cold trap pipe, the former and the carrier gas source's of sample concrete connection relation, for example the optional three-way valve that uses commonly on the market of controllable valve, six-way valve, diverter valve and ooff valve etc. no longer describe here any more.
Additionally, can also the utility model discloses a water trap for gas concentration sampling sets to the sampling device who is used for gas concentration sampling, directly utilizes control module's control function promptly, sets up fourth control mode in control module, moreover, fourth control mode: controlling the concentrated cold trap 3 to work in a desorption state, controlling a controllable valve on a pipeline, and leading carrier gas of a carrier gas source to be introduced into the concentrated cold trap pipe 300 so as to convey organic matters desorbed from the cold trap pipe of the concentrated cold trap to an analysis instrument or a sampling pipe, thereby realizing gas concentration sampling and automatic control of sample introduction of the analysis instrument.
The utility model provides a control module is the device that has switching signal output function and analog signal acquisition function, like integrated components and parts such as common PLC controller or singlechip on the market.
As shown in fig. 2 the utility model discloses a pipeline connection schematic diagram of gas concentration sampling device, control module is not shown, and this gas concentration sampling device concrete theory of operation is:
the carrier gas respectively obtains two paths of carrier gases with different pressure outputs after being subjected to two paths of pressure regulation, wherein the carrier gas with the output pressure of P1 is communicated to the port 2 of the switching valve 403 through the three-path switching valve and then is output through the port 1 thereof, so that the carrier gas is provided for the transmission line. The carrier gas with the output pressure of P2 reaches the 3 ports of the switching valve 402 through a switch valve, is connected to the 3 ports of the switching valve 403 through the 2 ports, and as the 3-6 ports of the switching valve 403 are communicated, the 6 ports are connected with one end of the concentrated cold trap tube 300, and meanwhile, the carrier gas with the output pressure of P2 is connected with the other end of the concentrated cold trap tube 300 through a switch valve and provides carrier gas for desorption and sample injection of the concentrated cold trap tube 300.
The sample gas is output to the port 2 of the six-way valve 401 through a multi-way selector valve, enters one end of the first cold trap pipe 100 from the port 1 of the six-way valve 401 and is connected, passes through the first cold trap pipe 100, then passes through the ports 1 and 2 of the switching valve 402, and the ports 3-6 of the switching valve 403, reaches the concentrated cold trap pipe 300, passes through the concentrated cold trap pipe 300, and then reaches the pump through the ports 5 and 6 of the switching valve 402, a switch valve and a flow controller. Since the first cold trap pipe 100 is in a-30 ℃ low-temperature adsorption state and filled with hydrophilic materials, moisture in the sample gas is absorbed, and meanwhile, the concentration cold trap pipe 300 is also in a-30 ℃ low-temperature adsorption state, the concentration cold trap pipe 300 concentrates the sample gas.
Then, the carrier gas with the output pressure P2 is output to the first cold trap tube 100 through the 6 th port and the 1 st port of the switching valve 401, and the carrier gas enters the second cold trap tube 200 after passing through the first cold trap tube 100, and is then discharged from the other end of the second cold trap tube 200. In the process, the first cold trap pipe 100 works in a heating state at 300 ℃, the second cold trap pipe 200 works in a low-temperature adsorption state at minus 30 ℃, carrier gas conveys the components desorbed from the first cold trap pipe 100 to the second cold trap pipe 200, and hydrophobic organic matter adsorbing materials are filled in the second cold trap pipe 200 to adsorb the organic matters desorbed from the first cold trap pipe 100, and meanwhile, the carrier gas brings the water desorbed from the first cold trap pipe 100 out of the second cold trap pipe 200, so that the water removal process is completed.
Then, the carrier gas with the output pressure P2 is output to the first cold trap pipe 100 and the second cold trap pipe 200 through the 6 ports and the 1 port of the switching valve 401, respectively, the first cold trap pipe 100 and the second cold trap pipe 200 are commonly connected to the 1 port of the switching valve 402, then reach the concentrated cold trap pipe 300 through the 2 ports of the switching valve 402 and the 3-6 ports of the switching valve 403, and reach the pump through the 5 ports and the 6 ports of the switching valve 402, a switch valve and a flow controller after passing through the concentrated cold trap pipe 300. In the process, the first cold trap pipe 100 and the second cold trap pipe 200 are controlled to work in a heating state, the concentration cold trap 3 works in a low-temperature adsorption state at minus 30 ℃, and the carrier gas can convey the organic matters desorbed from the first cold trap pipe 100 and the second cold trap pipe 200 to the concentration cold trap pipe 300 for concentration.
Moreover, after the water removal process of gas concentration sampling is completed, concentrated components need to be sent into an analysis instrument or a sample tube, the carrier gas with the output pressure P2 passes through the concentration cold trap tube 300, and is then output to the analysis instrument or the sample tube through the 6 port and the 1 port of the switching valve 403, and in addition, when the concentration of the concentrated sample is too high, because the 5 ports of the switching valve 403 are also connected with a switch valve and a flow regulating valve, the shunting of the high-concentration sample can be realized.
Claims (4)
1. A water removal device for gas concentration sampling is characterized by comprising a first cold trap, a second cold trap, a concentration cold trap and a control module; wherein the content of the first and second substances,
hydrophilic materials are filled in the cold trap pipe of the first cold trap;
the cold trap pipe of the second cold trap is filled with hydrophobic organic matter adsorption material;
three connection relations are included; wherein the content of the first and second substances,
the first connection relation: the control module is connected with the first cold trap, the concentration cold trap and a controllable valve on a pipeline, the first cold trap is connected with the concentration cold trap, and the control module is used for enabling sample gas of a sample gas source to sequentially pass through cold trap pipes of the first cold trap and the concentration cold trap; wherein the first cold trap and the concentrated cold trap work in a refrigerating state;
the second connection relation: the control module is connected with the first cold trap and the second cold trap and works in a refrigerating state, and controllable valves on pipelines are used for enabling carrier gas of a carrier gas source to sequentially pass through cold trap pipes of the first cold trap and the second cold trap; wherein the first cold trap works in a heating state, and the second cold trap works in a cooling state;
the third connection relationship is: the control module is connected with the first cold trap, the second cold trap and a controllable valve on a pipeline, and the first cold trap, the second cold trap and the concentrated cold trap are sequentially connected and used for enabling carrier gas of a carrier gas source to respectively pass through cold trap pipes of the first cold trap and the second cold trap and then enter the cold trap pipe of the concentrated cold trap; wherein the first cold trap and the second cold trap work in a heating state.
2. The water removal device for gas concentration sampling according to claim 1, wherein the first cold trap, the second cold trap and the concentration cold trap are each provided with a heating component, a refrigerating component and a temperature sensing element; and the control module controls the power of the heating component or the cooling component according to the temperature data detected by the temperature sensing elements of the first cold trap, the second cold trap and the concentration cold trap.
3. The water removal device for gas concentration sampling of claim 1, further comprising a pressure regulator for regulating the pressure of the carrier gas introduced by the carrier gas source.
4. A sample introduction device for gas concentration sampling, comprising the water removal device for gas concentration sampling according to any one of claims 1 to 3, and further comprising a fourth connection relationship: the control module is connected with the concentration cold trap and a controllable valve on a pipeline and is used for leading carrier gas of a carrier gas source to enter a cold trap pipe of the concentration cold trap so as to convey organic matters desorbed from the cold trap pipe of the concentration cold trap to an analysis instrument or a sampling pipe; the concentration cold trap works in a desorption state.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822034507.5U CN209841796U (en) | 2018-12-05 | 2018-12-05 | A water trap and sampling device for concentrated sampling of gas |
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| CN201822034507.5U CN209841796U (en) | 2018-12-05 | 2018-12-05 | A water trap and sampling device for concentrated sampling of gas |
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| CN209841796U true CN209841796U (en) | 2019-12-24 |
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| CN201822034507.5U Active CN209841796U (en) | 2018-12-05 | 2018-12-05 | A water trap and sampling device for concentrated sampling of gas |
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