CN112798358A - Material thermal volatilization gas sampling device for laboratory - Google Patents
Material thermal volatilization gas sampling device for laboratory Download PDFInfo
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- CN112798358A CN112798358A CN202011360548.9A CN202011360548A CN112798358A CN 112798358 A CN112798358 A CN 112798358A CN 202011360548 A CN202011360548 A CN 202011360548A CN 112798358 A CN112798358 A CN 112798358A
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- 238000005070 sampling Methods 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 58
- 230000004888 barrier function Effects 0.000 claims abstract description 49
- 230000000903 blocking effect Effects 0.000 claims abstract description 25
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 238000006073 displacement reaction Methods 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 27
- 229920000742 Cotton Polymers 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000009529 body temperature measurement Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 119
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
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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
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
-
- 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
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
-
- 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
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N2001/2244—Exhaled gas, e.g. alcohol detecting
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a material thermal volatilization gas sampling device for a laboratory, which is used for sampling volatile gas thermally cracked at a specific temperature, and comprises: displacing the gas source; the heating furnace is used for heating the material to be measured; a sample tube fixedly arranged on the heating furnace in a penetrating way; the upper end and the lower end of the sample tube are positioned outside the heating furnace; the lower end of the sample tube is communicated with the displacement gas source; the upper end of the sample tube is provided with a first blocking and ventilating piece; the lower end of the sample tube is provided with a second gas barrier; a sample accommodating space for accommodating a material to be tested is formed between the first air blocking and permeating piece and the second air blocking and permeating piece; a sampling tube; one end of the sampling tube is communicated with the upper end of the sample tube through a second pipeline; one end of the sampling tube is provided with a third air blocking and permeating part, and the other end of the sampling tube is provided with a fourth air blocking and permeating part; and a resin accommodating space for accommodating adsorption resin is formed between the third barrier air-permeable member and the fourth barrier air-permeable member.
Description
Technical Field
The invention relates to the field of gas sampling, in particular to a material thermal volatilization gas sampling device for a laboratory.
Background
Gas sampling is the process of collecting samples of atmospheric air or gases in the air. There are two types of collection methods: one is to make a large amount of air pass through a liquid absorbent or a solid adsorbent to enrich certain gases in the atmosphere, such as an air pumping method and a membrane filtering method. Another type is to collect the air containing the contaminants with containers (glass bottles, plastic bags, etc.).
The existing gas sampling device is basically applied to natural environment and used for collecting atmospheric components, and no device can be used for measuring volatile gas generated by heating and cracking certain solid materials at a specific temperature in a laboratory.
Disclosure of Invention
In view of the above-mentioned shortcomings, it is an object of the present invention to provide a material thermal volatilization gas sampling device for laboratory use, which facilitates sampling of volatilization gas for determining that certain solid materials are thermally cracked at a specific temperature in a laboratory.
In order to achieve the purpose, the invention adopts the following technical scheme:
a laboratory material thermally volatilized gas sampling device, comprising:
displacing the gas source;
the heating furnace is used for heating the material to be measured;
a sample tube fixedly arranged on the heating furnace in a penetrating way; the upper end and the lower end of the sample tube are positioned outside the heating furnace; the lower end of the sample tube is communicated with the displacement gas source; the upper end of the sample tube is provided with a first blocking and ventilating piece; the lower end of the sample tube is provided with a second gas barrier; a sample accommodating space for accommodating a material to be tested is formed between the first air blocking and permeating piece and the second air blocking and permeating piece;
a sampling tube; one end of the sampling tube is communicated with the upper end of the sample tube through a second pipeline; one end of the sampling tube is provided with a third air blocking and permeating part, and the other end of the sampling tube is provided with a fourth air blocking and permeating part; a resin accommodating space for accommodating adsorption resin is formed between the third barrier air-permeable member and the fourth barrier air-permeable member; at least one of the first barrier air-permeable member, the second barrier air-permeable member, the third barrier air-permeable member and the fourth barrier air-permeable member comprises a metal mesh arranged at the end part and medium filter cotton filled at the end part; the medium filter cotton is soaked with gas adsorption liquid and/or gas indicator liquid.
In a preferred embodiment, at least two of the first barrier air-permeable member, the second barrier air-permeable member, the third barrier air-permeable member and the fourth barrier air-permeable member are soaked with different liquids.
As a preferred embodiment, the laboratory material thermal volatilization gas sampling device further comprises a console; the heating furnace is supported on the control platform; the console is provided with an air inlet and an air outlet; the gas inlet is connected with the displacement gas source through a first pipeline; the console is provided with a first gas flow controller for controlling the gas flow; the gas outlet is communicated with the lower end of the sample tube.
In a preferred embodiment, the first pipeline is further provided with a second gas flow controller; the control accuracy of the second gas flow controller is lower than the control accuracy of the first gas flow controller.
In a preferred embodiment, the first gas flow controller is a gas mass flow controller; the second gas flow controller is a rotameter; the console is provided with a flow display and a flow adjusting part which are connected with the first gas flow controller.
As a preferred embodiment, a temperature measuring member for measuring a heating temperature and a heating member for heating the temperature are provided in the heating furnace; the console is provided with a temperature display controller connected with the temperature measuring part and the heating part.
In a preferred embodiment, the temperature measuring member is a thermocouple element; the heating furnace is a sintering furnace.
As a preferred embodiment, a wiring outlet electrically connected with the temperature measuring part and the heating part is arranged on the side wall of the heating furnace; the control console is provided with a wiring inlet which is electrically connected with the temperature display controller; the wiring outlet is connected with the wiring inlet through a cable.
In a preferred embodiment, the temperature display controller includes a temperature display and a temperature adjustment unit.
In a preferred embodiment, the displacement gas source is an air compressor.
Has the advantages that:
according to the material thermal volatilization gas sampling device for the laboratory, provided by the embodiment of the invention, high-pressure gas generated by a displacement gas source is introduced into the heated sample tube, the heated and volatilized thermal volatilization gas is driven out of the sample tube into the sampling tube, and the thermal volatilization gas is adsorbed by the adsorption resin in the sampling tube, so that the sampling of the thermal volatilization gas under the laboratory condition is completed. Thus, the material thermal volatilization gas sampling device for the laboratory can sample volatilization gas which is used for measuring certain solid materials in the laboratory and is thermally cracked at a specific temperature.
Specific embodiments of the present invention are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the invention may be employed. It should be understood that the embodiments of the invention are not so limited in scope.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a schematic diagram of a laboratory material thermal volatilization gas sampling device according to one embodiment of the invention;
FIG. 2 is a schematic view of the console and furnace of FIG. 1;
fig. 3 is a cross-sectional view of fig. 2.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of protection of the present invention.
It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1 to 3, an embodiment of the present invention provides a device for sampling material thermal volatilization gas for a laboratory, comprising: a displacement gas source 6; a heating furnace 1 for heating a material to be measured; a sample tube 4 fixedly arranged on the heating furnace 1 in a penetrating way; sampling tube 7.
Wherein the upper end and the lower end of the sample tube 4 are positioned outside the heating furnace 1. The lower end of the sample tube 4 is communicated with the displacement gas source 6. The upper end of the sample tube 4 is provided with a first blocking and ventilating piece. The lower end of the sample tube 4 is provided with a second gas barrier. And a sample containing space for containing the material to be tested is formed between the first barrier air-permeable piece and the second barrier air-permeable piece.
One end of the sampling tube 7 is communicated with the upper end of the sample tube 4 through a second pipeline (the number is also 8, and the material specification of the sampling tube can be considered to be consistent with that of the first pipeline). One end of the sampling tube 7 is provided with a third barrier air-permeable member, and the other end is provided with a fourth barrier air-permeable member. And a resin accommodating space for accommodating adsorption resin is formed between the third barrier air-permeable member and the fourth barrier air-permeable member.
The laboratory that this embodiment provided lets in heated sample tube 4 with the produced high-pressure gas of displacement air supply 6 in the material thermal volatilization gas sampling device that utilizes, and the thermal volatilization gas that will send the heating drives out the sample tube from sample tube 4 in, and the adsorption resin in utilizing the sample tube adsorbs the thermal volatilization gas, accomplishes the sampling of thermal volatilization gas under the laboratory condition. Thus, the material thermal volatilization gas sampling device for the laboratory can sample volatilization gas which is used for measuring certain solid materials in the laboratory and is thermally cracked at a specific temperature.
The sampling tube 7 of this embodiment adopts the adsorption resin to carry out the sample of thermal volatilization gas, both can adsorb volatile organic gas, can also elute the gas that adsorbs in organic solvent such as petroleum ether, and then can carry out the chromatogram mass spectrum detection, judge organic gas composition.
In this embodiment, the material to be tested is a solid sample, and in order to prevent the material to be tested from falling, blocking and air-permeable members are respectively disposed at two ends of the sample tube 4 and the sampling tube 7, so as to allow the material to be tested not to fall, but also allow gas to pass, thereby ensuring the smooth operation of the experiment.
In particular, the first and second gas-barrier members allow the passage of gas and prevent the leakage of the material to be tested from the sample tube 4. Wherein the material to be tested may be filled between the first barrier gas permeable member and the second barrier gas permeable member. Like the first and second gas-barrier members, the third and fourth gas-barrier members allow gas to pass therethrough and prevent the adsorbent resin from leaking out of the sampling tube 7. Wherein the adsorption resin may be filled between the first barrier gas permeable member and the second barrier gas permeable member.
At least one of the first barrier air-permeable member, the second barrier air-permeable member, the third barrier air-permeable member and the fourth barrier air-permeable member comprises a metal mesh arranged at the end part and medium filter cotton filled at the end part; the medium filter cotton is soaked with gas adsorption liquid and/or gas indicator liquid. Considering that the temperature is higher when the sample tube is heated, in order to improve the experimental safety, the medium filter cotton can be glass cotton or quartz cotton and other non-combustible porous media. Wherein, the medium filter cotton can filter to the gas component that does not need or carry out the preliminary testing to the gas component. Of course, when the particle size of the particles to be measured is large, the end of the sample tube or the sampling tube can be plugged by the wound copper mesh to realize the porous plugging effect.
In this embodiment, when the media filter cotton is soaked with the gas adsorption liquid, the gas adsorption liquid thereon adsorbs the reactive gas component in the passing gas, and then only the gas component part desired to be sampled passes through. For example, the gas adsorption liquid may be a sodium hydroxide or calcium hydroxide solution, so that the carbon dioxide component in the gas passing through can be adsorbed and removed.
In further embodiments, the media filter cotton may also serve as a gas composition indicator to detect whether a target detection gas composition is present for the gas composition passing therethrough. For example, the gas indicator liquid may be a purple litmus sample liquid, and the degree of color change of the medium filter cotton after the gas passes through the liquid indicator liquid may be used to indicate that the gas contains carbon dioxide, or the concentration of carbon dioxide in the gas passing through the liquid indicator liquid may be estimated by the degree of color change of the medium filter cotton.
Further, the liquid soaked by the medium filter cotton of at least two of the first air-permeable blocking piece, the second air-permeable blocking piece, the third air-permeable blocking piece and the fourth air-permeable blocking piece is different. For example: the first blocking and air-permeable piece and the second blocking and air-permeable piece are different in liquid soaked by the medium filter cotton, the medium filter cotton of the first blocking and air-permeable piece can be soaked with a calcium hydroxide solution, and the medium filter cotton of the second blocking and air-permeable piece can be soaked with a purple litmus test solution. Of course, the media filter cotton in the first barrier air-permeable member, the second barrier air-permeable member, the third barrier air-permeable member and the fourth barrier air-permeable member may not contain the gas absorption liquid and the gas indicator liquid, and the invention is not limited solely.
The first barrier vent, the second barrier vent, the third barrier vent, and the fourth barrier vent may each comprise a metal mesh and a media filter cotton. The medium filter cotton is plugged at the pipe end in a mode of filling and plugging in the port pipe at the pipe end, and the metal net is fixed on the outer side of the medium filter cotton. Preferably, the metal mesh may be a copper mesh. In the case of a gas indicator liquid carried by a media filter cotton, the sample tube 4 or the sampling tube 7 may be of a transparent material. In the present embodiment, the sample tube 4 may be a steel tube. The sampling tube 7 may also be a steel tube, although in other embodiments the sampling tube 7 may be a clear glass tube.
In a preferred embodiment, to achieve the gas indicating or removing function, the third barrier air-permeable member and/or the fourth barrier air-permeable member may include a metal mesh and a medium filter cotton attached with indicator liquid or adsorption liquid, and the first barrier air-permeable member and the second barrier air-permeable member have the metal mesh and a medium filter cotton not attached with indicator liquid or adsorption liquid.
In this embodiment, the laboratory material thermal volatilization gas sampling device further comprises a console 14. The heating furnace 1 is supported on the console 14. The console 14 has an air inlet 9 and an air outlet. The gas inlet 9 is connected with the displacement gas source 6 through a first pipeline 8. The console 14 is provided with a first gas flow controller that controls the flow of gas. The first gas flow controller is communicated between the gas inlet 9 and the gas outlet so as to control the flow of the gas supplied to the sample tube 4, thereby controlling the flow of the gas substances volatilized by pyrolysis of the sample (material to be tested) in the sample tube 4 so as to be fully displaced and blown into the sampling tube 7. The air outlet is communicated with the lower end of the sample tube 4.
The console 14 has a mounting platform, and the heating furnace 1 is fixedly supported on the mounting platform of the console 14. Specifically, the heating furnace 1 may be fixed to the console 14 by a welding bracket 13. The sample tube 4 vertically passes through the heating furnace 1. The main body of the heating furnace 1 is cylindrical, and the sample tube 4 can be fixedly inserted into the central axis of the heating furnace 1.
In order to further realize the control of the displacement gas flow, a second gas flow controller is also arranged on the first pipeline 8. The control accuracy of the second gas flow controller is lower than the control accuracy of the first gas flow controller. The second gas flow controller can realize coarse adjustment of gas flow, and the first gas flow controller is used for fine adjustment of gas flow.
Specifically, the first gas flow controller is a gas mass flow controller 12. The gas mass flow controller 12 may be disposed inside the console 14. The outlet end of the gas mass flow controller 12 is connected with an outlet pipe 16, and the upper end of the outlet pipe 16 extends out of the mounting platform of the console 14 to form an air outlet. The second gas flow controller is a rotameter 5. The console 14 is provided with a flow indicator 2 connected to the first gas flow controller. The flow display 2 may include a flow display and a flow adjustment portion. The flow rate adjusting unit may be a knob or a button (e.g., a power switch) and the operator adjusts and controls the flow rate of the gas to be input to the sample tube 4. The flow display may display the flow of gas supplied to the sample tube 4. For the convenience of flow control, the rotameter can also be connected with a flow display instrument 2 through a wire, and the rotameter can be switched on and off or subjected to flow regulation control by using the flow display instrument 2.
In this embodiment, the displacement gas source 6 is an air compressor. The first conduit 8 comprises a first vent pipe connected between the air compressor and the rotameter 5, and a second vent pipe connected between the rotameter 5 and the air inlet 9 of the console 14. In other embodiments, the displacement gas source 6 may also be a high pressure gas cylinder, and the invention is not limited solely thereto.
In the present embodiment, the heating furnace 1 is provided therein with a temperature measuring member for measuring a heating temperature, and a heating member for heating the temperature. The console 14 is provided with a temperature display controller 3 connected to the temperature measuring member and the heating member. Specifically, the temperature measuring member is a thermocouple element 15. The heating furnace 1 is a sintering furnace, and specifically, the sintering furnace can be a programmable sintering furnace. The heating element can be a resistance wire inside the sintering furnace.
And a wiring outlet 10 electrically connected with the temperature measuring part and the heating part is arranged on the side wall of the heating furnace 1. And the control console 14 is provided with a wiring inlet 11 electrically connected with the temperature display controller 3. The connection outlet 10 and the connection inlet 11 are connected through a cable. In order to adjust the heating temperature of the heating furnace 1, the temperature display controller 3 includes a temperature display and a temperature adjustment unit.
As shown in fig. 1 to 3, the temperature display controller 3 (for example, a sintering furnace face), the flow rate display, and the flow rate adjusting portion, the gas mass flow controller 12 are installed in the console 14 and electrically connected. The air compressor is connected with one end of the first vent pipe in an inserting mode, the other end of the first vent pipe is connected with the air inlet end of the rotameter 5 in an inserting mode, and then the air outlet end of the rotameter 5 is connected with one end of the second vent pipe in an inserting mode. The other end of the second vent tube is then inserted into the air inlet 9 of the console 14. A programmable sintering furnace is arranged above the control platform 14. The programmable sintering furnace is fixed on a control console 14 through a welding bracket 13, then the thermocouple (element) is placed in the programmable sintering furnace and sealed, then the temperature display controller 3 and the thermocouple element 15 are electrically connected through a wire inlet and a wire outlet, finally a sample tube 4 is inserted into the center of the programmable sintering furnace, one end of a second pipeline is connected to the upper part of the sample tube 4, and the other end of the second pipeline is connected to the sampling tube 7. Specifically, the sample tube 4 may be a steel tube having a tube diameter of DN8 and a length of 20 cm. The sampling tube 7 can be a steel tube with the tube diameter of DN6 and the length of 15 cm. The vent pipe may be a 6 rubber hose.
The sampling flow using the material thermal volatilization gas sampling device for the laboratory of the embodiment is as follows:
(1) the material to be tested was cut into a 2X 0.2cm strip and placed in a sample tube 4, and then the sample tube 4 (a steel tube having a tube diameter of DN8 and a length of 20 cm) was attached to the heating furnace 1.
(2) And the adsorption resin capable of adsorbing organic gas is loaded into a sampling pipe 7 (steel pipe with the pipe diameter of DN6 and the length of 15 cm), and sealed with a clean copper net and cotton to prevent the adsorption resin from leaking, and the adsorption resin is labeled and installed at the tail end of the second pipeline.
(3) And second pipelines respectively connecting the air compressor and the rotameter 5, the rotameter 5 and the gas mass flow controller 12, and the sample tube 4 and the sampling tube 7.
(4) And turning on a power switch of the temperature display controller 3 to heat the interior of the heating furnace 1 to heat the sample tube 4. The heating temperature of the heating furnace 1 is firstly raised to 130 ℃ for preheating, then raised to the target temperature, and the heating temperature is kept through the temperature keeping key of the temperature display controller 3.
When the temperature reaches the target temperature, the gas mass flow controller 12 on the flow display instrument 2 and the adjusting switch (adjusting knob) of the rotor flow meter 5 are turned on, the air compression pump is turned on and maintained for 20s, the rotor flow meter 5 is roughly adjusted, then the flow display instrument 2 is finely adjusted, and the flow displayed by the flow display instrument 2 is enabled to reach 0.5cm3And/min, closing the air compressor. And simultaneously recording the time, and starting the air compressor once every 10min to maintain the flow of the displacement gas. The sampling was completed by timing 30 minutes. The gas mass flow controller 12 is closed and the sampling tube 7 is removed. And (3) closing the sintering furnace, the air compressor and the rotor flow meter 5 in sequence, and taking out the sampling tube 7 to replace the sample after the sampling tube is cooled to the room temperature.
Any numerical value recited herein includes all values from the lower value to the upper value, in increments of one unit, provided that there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of a component or a value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, it is intended that equivalents such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also expressly enumerated in this specification. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are only examples of what is intended to be explicitly recited, and all possible combinations of numerical values between the lowest value and the highest value that are explicitly recited in the specification in a similar manner are to be considered.
Unless otherwise indicated, all ranges include the endpoints and all numbers between the endpoints. The use of "about" or "approximately" with a range applies to both endpoints of the range. Thus, "about 20 to about 30" is intended to cover "about 20 to about 30", including at least the endpoints specified.
All articles and references disclosed, including patent applications and publications, are hereby incorporated by reference for all purposes. The term "consisting essentially of …" describing a combination shall include the identified element, ingredient, component or step as well as other elements, ingredients, components or steps that do not materially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe combinations of elements, components, or steps herein also contemplates embodiments that consist essentially of such elements, components, or steps. By using the term "may" herein, it is intended to indicate that any of the described attributes that "may" include are optional.
A plurality of elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, ingredient, component or step is not intended to foreclose other elements, ingredients, components or steps.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are hereby incorporated by reference for all purposes. The omission in the foregoing claims of any aspect of subject matter that is disclosed herein is not intended to forego such subject matter, nor should the inventors be construed as having contemplated such subject matter as being part of the disclosed subject matter.
Claims (10)
1. A laboratory is with material thermal volatilization gas sampling device which characterized in that includes:
displacing the gas source;
the heating furnace is used for heating the material to be measured;
a sample tube fixedly arranged on the heating furnace in a penetrating way; the upper end and the lower end of the sample tube are positioned outside the heating furnace; the lower end of the sample tube is communicated with the displacement gas source; the upper end of the sample tube is provided with a first blocking and ventilating piece; the lower end of the sample tube is provided with a second gas barrier; a sample accommodating space for accommodating a material to be tested is formed between the first air blocking and permeating piece and the second air blocking and permeating piece;
a sampling tube; one end of the sampling tube is communicated with the upper end of the sample tube through a second pipeline; one end of the sampling tube is provided with a third air blocking and permeating part, and the other end of the sampling tube is provided with a fourth air blocking and permeating part; a resin accommodating space for accommodating adsorption resin is formed between the third barrier air-permeable member and the fourth barrier air-permeable member; at least one of the first barrier air-permeable member, the second barrier air-permeable member, the third barrier air-permeable member and the fourth barrier air-permeable member comprises a metal mesh arranged at the end part and medium filter cotton filled at the end part; the medium filter cotton is soaked with gas adsorption liquid and/or gas indicator liquid.
2. The laboratory material thermally volatilized gas sampling device of claim 1, wherein at least two of the first, second, third, and fourth barrier plenums are different in liquid wetted by the media filter batts.
3. The laboratory material thermally volatilized gas sampling device of claim 1 further comprising a console; the heating furnace is supported on the control platform; the console is provided with an air inlet and an air outlet; the gas inlet is connected with the displacement gas source through a first pipeline; the console is provided with a first gas flow controller for controlling the gas flow; the gas outlet is communicated with the lower end of the sample tube.
4. The laboratory material thermally volatilized gas sampling device of claim 3 wherein a second gas flow controller is further provided on the first conduit; the control accuracy of the second gas flow controller is lower than the control accuracy of the first gas flow controller.
5. The laboratory material thermally volatilized gas sampling device of claim 4, wherein the first gas flow controller is a gas mass flow controller; the second gas flow controller is a rotameter; the console is provided with a flow display and a flow adjusting part which are connected with the first gas flow controller.
6. The laboratory material thermally volatilized gas sampling device as recited in claim 3, wherein a temperature measuring member for measuring a heating temperature and a heating member for heating the temperature are provided in the heating furnace; the console is provided with a temperature display controller connected with the temperature measuring part and the heating part.
7. The laboratory material thermally volatilized gas sampling device of claim 6, wherein the temperature measurement member is a thermocouple element; the heating furnace is a sintering furnace.
8. The laboratory material thermally volatile gas sampling device as set forth in claim 6, wherein a wiring outlet electrically connected to said temperature measuring member and said heating member is provided on a side wall of said heating furnace; the control console is provided with a wiring inlet which is electrically connected with the temperature display controller; the wiring outlet is connected with the wiring inlet through a cable.
9. The laboratory material thermally volatilized gas sampling device of claim 8, wherein the temperature display controller includes a temperature display and a temperature adjustment section.
10. The laboratory material thermally volatilized gas sampling device of claim 1, wherein the displacement gas source is an air compressor.
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Application publication date: 20210514 |