In-situ online gas detection device and detection system based on electron paramagnetism

Abstract

The utility model relates to an in-situ online gas detection device and system based on electron paramagnetism. The in-situ online gas detection device comprises a base, an EPR paramagnetic spectrometer, a reaction tank assembly and a gas path assembly, the EPR paramagnetic wave spectrometer is arranged on the base; the reaction tank assembly is mounted on the EPR paramagnetic wavelength dispersive spectrometer and comprises a fixed seat, a bushing, a sample tube and a gas guide tube; the gas circuit assembly comprises a reaction tank and a vacuum pump arranged on two sides of the base, the reaction tank is connected with the gas inlet through a gas inlet pipe, and the vacuum pump is connected with the exhaust hole through an exhaust pipe; according to the detection device, the gas path assembly and the reaction tank assembly are arranged to form the gas detection device capable of introducing gas into the EPR paramagnetic spectrometer for detection; in addition, the detection device can be used for detecting solid or liquid samples, particularly can be used for creating air environments such as oxygen filling, inert gas filling or vacuumizing for the solid or liquid samples, and can realize in-situ testing; the whole device is easy to operate, convenient to install and maintain and high in practicability.

Description

TECHNICAL FIELD

[0001] The utility model relates to gas detection device technical field especially is to point to in situ online gas detection device and detection system based on electron paramagnetic. BACKGROUND

[0002] Electron paramagnetic resonance (EPR) is a kind of magnetic resonance technology originated from the magnetic moment of unpaired electron, and is an important tool for studying the unpaired electron state of compound or mineral, which can be used to detect the unpaired electron contained in the atoms or molecules of the substance from qualitative and quantitative aspects, and explore the structural characteristics of its surrounding environment. Electron paramagnetic resonance is also called electron spin resonance (EPR), and its basic principle is that electron is a basic particle with certain mass and negative charge, which can perform two kinds of motion: one is motion on the orbit around the atomic nucleus, and the other is spin made by its own central axis. Since the electron motion produces torque, current and magnetic moment are generated in the motion. In the external magnetic field, the degenerate electron spin energy level will be split, and if a suitable frequency electromagnetic wave is added in the direction perpendicular to the external magnetic field, the electron in the low spin energy level can absorb electromagnetic wave energy and jump to the high energy level, thereby producing electron paramagnetic resonance absorption phenomenon.

[0003] The electron paramagnetic resonance spectrometer is usually composed of radiation source, resonance cavity, sample holder, signal receiving, amplifier and recorder, etc. The EPR spectrum of mineral can provide information such as lattice position, valence state, local symmetry, concentration and crystal field parameters of paramagnetic center impurities in mineral, so as to study the ground state electron structure and chemical bond properties, and explain some physical properties of mineral. The electron paramagnetic resonance spectrometer is mainly applied to study paramagnetic impurity ions (concentration less than 1%) in mineral, such as isomorphous substitution of over elements ions and rare earth element ions, order-disorder, chemical bond and lattice parameters and local symmetry, and study the type, concentration and properties of electron-hole center related to point defects. The electron paramagnetic resonance spectrum also plays an important role in the study of mineral color.

[0004] The existing commercial electron paramagnetic resonance spectrometer can usually only be used for detection of liquid or solid samples, and cannot detect gas samples. Moreover, it cannot create a corresponding gas environment for the sample during its reaction process, cannot realize in-situ detection, and cannot truly detect the electronic structure of the substance and the chemical reaction process. UTILITY MODEL CONTENT

[0005] Therefore, the utility model solves the problems in the prior art that the commercial electron paramagnetic resonance spectrometer can usually only be used for detection of liquid or solid samples, cannot detect gas samples, and cannot create a corresponding gas environment for the sample during its reaction process, cannot realize in-situ detection, and cannot truly detect the electronic structure of the substance and the chemical reaction process.

[0006] To solve the above technical problems, the utility model provides a kind of in situ online gas detection device based on electron paramagnetic resonance;

[0007] Base;

[0008] EPR paramagnetic spectrometer, the EPR paramagnetic spectrometer is arranged on the base, and the EPR paramagnetic spectrometer includes internal microwave resonant cavity;

[0009] Reaction cell assembly, the reaction cell assembly is installed on the EPR paramagnetic spectrometer, the reaction cell assembly includes fixed seat, bushing, sample tube and gas guide pipe, one end of the fixed seat is provided with accommodating groove, the other end is provided with gas inlet hole communicated with the accommodating groove, and the side surface of the fixed seat is provided with gas outlet hole, a plurality of flow guide diffusion holes communicated with the accommodating groove are formed in the inner wall of the gas outlet hole, the bushing is sleeved on the one end of the fixed seat provided with accommodating groove, the sample tube is a pipe structure with one end sealed, the sealed end of the sample tube extends into the microwave resonant cavity, the open end of the sample tube extends into the accommodating groove through the bushing, the gas guide pipe is arranged in the sample tube, one end of the gas guide pipe is connected with the gas inlet hole, and the other end extends to the sealed end of the sample tube;

[0010] Gas path assembly, the reaction tank and vacuum pump are arranged on the two sides of the base respectively, the output end of the reaction tank is connected with the gas inlet hole through gas inlet pipe, and the vacuum pump is connected with the gas outlet hole through gas outlet pipe.

[0011] In an embodiment of the utility model, pressure regulating valve group is arranged between the reaction tank and the gas inlet pipe.

[0012] In an embodiment of the utility model, quick coupler is arranged on the gas inlet hole and the gas outlet hole, and the gas inlet pipe and the gas outlet pipe are connected with the gas inlet hole and the gas outlet hole respectively through the quick coupler.

[0013] In an embodiment of the utility model, the base includes base main body in cuboid shape, the base main body is horizontally arranged, and two support frames in groove shape are symmetrically connected to the two ends of the base main body, the EPR paramagnetic spectrometer is arranged on the base main body, and the reaction tank and the vacuum pump are arranged in the two support frames respectively.

[0014] In an embodiment of the utility model, mounting hole communicated with the microwave resonant cavity is formed in the EPR paramagnetic spectrometer, mounting sleeve is coaxially arranged in the mounting hole, and the sample tube extends into the microwave resonant cavity through the mounting sleeve.

[0015] In an embodiment of the utility model, the fixed seat is cylindrical structure, one end of the bushing is provided with the circular groove which matches with the diameter of the fixed seat and is sleeved on one end of the fixed seat through the circular groove, and the bottom of the circular groove is provided with the through hole, the sample tube extends to the accommodating groove through the through hole.

[0016] In an embodiment of the utility model, the sample tube is sleeved with the sealing ring which is compressed between the fixed seat and the bushing.

[0017] In an embodiment of the utility model, the air inlet hole is coaxially provided with the sealing sleeve, and one end of the air guide pipe is sealingly connected with the air inlet hole through the sealing sleeve.

[0018] In an embodiment of the utility model, the sample tube and the air guide pipe are both quartz tubes.

[0019] A detection system comprises the in-situ online gas detection device based on electron paramagnetism as claimed in any one of the preceding claims.

[0020] Compared with the prior art, the above technical scheme of the utility model has the following advantages:

[0021] The in-situ online gas detection device based on electron paramagnetism and the detection system, comprising a base, an EPR paramagnetic spectrometer, a reaction cell assembly and a gas path assembly, the EPR paramagnetic spectrometer is arranged on the base, the reaction cell assembly is installed on the EPR paramagnetic spectrometer, the reaction cell assembly comprises a fixed seat, a bushing, a sample tube and an air guide pipe, one end of the fixed seat is provided with an accommodating groove, the other end is provided with an air inlet hole which is communicated with the accommodating groove, and a plurality of flow guide diffusion holes which are communicated with the accommodating groove are arranged on the inner wall of the air exhaust hole, the bushing is sleeved on one end of the fixed seat provided with the accommodating groove, the sample tube is a pipe structure with one end sealed, the sealed end of the sample tube extends into the microwave resonant cavity, one end of the air guide pipe is connected with the air inlet hole, and the other end extends to the sealed end of the sample tube, the gas path assembly comprises a reaction tank and a vacuum pump which are arranged on the two sides of the base respectively, the output end of the reaction tank is connected with the air inlet hole through an air inlet pipe, and the vacuum pump is connected with the air exhaust hole through an air exhaust pipe.The detection device is provided with the gas path assembly and the reaction cell assembly, so that the gas detection device for detecting the gas in the EPR paramagnetic spectrometer can be formed, and the detection device can also detect solid or liquid samples, especially can create an air environment such as full of oxygen, inert gas or vacuum for the solid or liquid samples, so that in-situ testing can be realized, the whole device is simple to operate, easy to install and maintain, and has high practicability. BRIEF DESCRIPTION OF DRAWINGS

[0022] In order to make the content of the utility model more easily be clearly understood, the following according to the specific embodiment of the utility model and combining with the drawings, the utility model is further explained in detail, wherein

[0023] Figure 1 It is the schematic diagram of the whole structure of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model;

[0024] Figure 2 It is the structural schematic diagram of the reaction pool assembly of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model;

[0025] Figure 3 It is the exploded view of the reaction pool assembly of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model;

[0026] Figure 4 It is the structural schematic diagram of the first visual angle of the fixing seat of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model;

[0027] Figure 5 It is the structural schematic diagram of the second visual angle of the fixing seat of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model;

[0028] Figure 6 It is the structural schematic diagram of the bushing of the in-situ online gas detection device based on electron paramagnetism of the preferred embodiment of the utility model.

[0029] Description of the drawing of the specification: 1, base;2, EPR paramagnetic spectrometer;3, reaction pool assembly;31, fixing seat;311, containing groove;312, gas inlet hole;313, exhaust hole;314, flow guide diffusion hole;32, bushing;33, sample tube;34, gas guide pipe;35, sealing ring;4, gas path assembly;41, reaction tank;42, vacuum pump;43, gas inlet pipe;44, exhaust pipe;5, pressure regulating valve group. Specific implementation

[0030] The utility model is further explained in combination with the drawings and specific embodiments, so that the person skilled in the art can better understand the utility model and can be implemented, but the embodiment is not as the limitation of the utility model.

[0031] Embodiment one

[0032] Referring to Figures 1-6 The utility model discloses a kind of in-situ online gas detection devices based on electron paramagnetism, including,

[0033] Base 1;

[0034] The EPR paramagnetic spectrometer 2 is arranged on the base 1, and the EPR paramagnetic spectrometer 2 comprises an internal microwave resonance cavity;

[0035] The reaction pool assembly 3 is arranged on the EPR paramagnetic spectrometer 2, and the reaction pool assembly 3 comprises a fixing base 31, a bushing 32, a sample tube 33 and a gas guide pipe 34, one end of the fixing base 31 is provided with a containing groove 311, the other end of the fixing base 31 is provided with a gas inlet hole 312 which is communicated with the containing groove 311, and a plurality of gas outlet holes 313 are arranged on the side surface of the fixing base 31, and a plurality of flow guide diffusion holes 314 which are communicated with the containing groove 311 are arranged on the inner wall of the gas outlet holes 313, the bushing 32 is arranged on one end of the fixing base 31 which is provided with the containing groove 311, the sample tube 33 is a tube structure with one end sealed, the sealed end of the sample tube 33 extends into the microwave resonance cavity, the open end of the sample tube 33 extends into the containing groove 311 through the bushing 32, and the gas guide pipe 34 is arranged in the sample tube 33, one end of the gas guide pipe 34 is connected with the gas inlet hole 312, and the other end of the gas guide pipe 34 extends to the sealed end of the sample tube 33.

[0036] The gas path assembly 4 comprises a reaction tank 41 and a vacuum pump 42 which are arranged on the two sides of the base 1 respectively, the output end of the reaction tank 41 is connected with the gas inlet hole 312 through a gas inlet pipe 43, and the vacuum pump 42 is connected with the gas outlet hole 313 through a gas outlet pipe 44.

[0037] The gas detection device can pass the gas into the microwave resonance cavity of the EPR paramagnetic spectrometer 2 for detection, and the gas pressure and concentration passed into the reaction pool assembly 3 can be regulated and controlled, the detection device can detect the gas sample and also can detect the solid or liquid sample, especially can create an air environment such as full of oxygen, inert gas or vacuum extraction for the solid or liquid sample, and in-situ testing can be realized, the whole device is simple in operation, convenient in installation and maintenance, and has high practicability.

[0038] Referring to Figure 1 Further, the reaction tank 41 and the gas inlet pipe 43 are provided with a pressure regulating valve group 5, the gas pressure passed into the reaction pool assembly 3 can be detected and adjusted in real time through the pressure regulating valve group 5, the gas sample concentration can reach the requirement, the gas pressure can also be ensured to be not more than the pressure resistance requirement of the reaction pool assembly 3, and the safety of the detection process is ensured.

[0039] Referring to Figure 2 and Figure 3As shown, further, the air inlet hole 312 and the air outlet hole 313 are provided with quick couplings, and the air inlet pipe 43 and the air outlet pipe 44 are connected to the air inlet hole 312 and the air outlet hole 313 respectively through the quick couplings. It is conceivable that the quick couplings can realize quick mounting and dismounting of the air inlet pipe 43 and the air outlet pipe 44, thereby improving the efficiency of installation and maintenance.

[0040] Referring to Figure 1 As shown, further, the base 1 includes a cuboid base body, the base body is horizontally arranged, and two slot-shaped support frames are symmetrically connected to the two ends of the base body, the EPR paramagnetic spectrum instrument 2 is arranged on the base body, and the reaction tank 41 and the vacuum pump 42 are arranged in the two support frames respectively.

[0041] Further, the EPR paramagnetic spectrum instrument 2 is provided with a mounting hole communicating with the microwave resonance cavity, and a mounting sleeve is coaxially arranged in the mounting hole, and the sample tube 33 extends into the microwave resonance cavity through the mounting sleeve. Specifically, the EPR paramagnetic spectrum instrument 2 is provided with a clamp for fixing the reaction cell assembly 3, the reaction cell assembly 3 is stably mounted on the EPR paramagnetic spectrum instrument 2 through the clamp, and the sample tube 33 of the reaction cell assembly 3 extends into the microwave resonance cavity.

[0042] Referring to Figures 3-6 As shown, further, the fixing seat 31 is in a cylindrical structure, one end of the bushing 32 is provided with a circular groove matching the diameter of the fixing seat 31 and is sleeved on one end of the fixing seat 31 through the circular groove, and a through hole is formed in the bottom of the circular groove, and the sample tube 33 extends into the accommodating groove 311 through the through hole. Specifically, the accommodating groove 311 is a circular groove corresponding to the shape and size of the sample tube 33, the open end of the sample tube 33 extends into the accommodating groove 311 through the through hole on the bushing 32, and a sealing ring 35 is sleeved on the sample tube 33 at the slot opening of the accommodating groove 311, and the sealing ring 35 is compressed between the fixing seat 31 and the bushing 32 after the bushing 32 is sleeved on the fixing seat 31, thereby ensuring the sealing performance of the connection position.

[0043] Further, the sample tube 33 is sleeved with the sealing ring 35 compressed between the fixing seat 31 and the bushing 32, and the sealing ring 35 is a high-temperature-resistant sealing ring.

[0044] Further, a sealing sleeve is coaxially arranged in the air inlet hole 312, and one end of the gas guide pipe 34 is sealingly connected to the air inlet hole 312 through the sealing sleeve.

[0045] Further, the sample tube 33 and the gas guide pipe 34 are both quartz tubes.

[0046] Working process:

[0047] Detection of gaseous reactants: first, the gaseous mixed reactants are introduced into the reaction tank 41, and the preparation of the gaseous sample is completed; then the vacuum pump 42 is started, and the exhaust pipe 44, the reaction cell assembly 3 and the gas inlet pipe 43 are vacuumized, and after a certain negative pressure is reached, the vacuum pump 42 is stopped, the valve of the reaction tank 41 is opened, and the gaseous sample is filled into the reaction cell assembly 3 through the gas inlet pipe 43, and in the filling process, the gaseous sample enters the sample tube 33 through the gas inlet hole 312 and the gas guide pipe 34 in turn, and the gaseous sample gradually accumulates from the bottom of the sample tube 33 (i.e. the sealed end of the sample tube 33), until the sample tube 33 is filled with the gaseous sample, and in the filling process, the pressure regulating valve group 5 is adjusted in real time, so that the reaction cell assembly 3 reaches the predetermined pressure, and then the EPR paramagnetic spectrometer 2 is started to scan and detect the gaseous sample.

[0048] Detection of solid or liquid samples: first, the solid or liquid sample is filled into the sample tube 33, and after the filling is completed, the reaction cell assembly 3 is installed on the EPR paramagnetic spectrometer 2; then oxygen or inert gas is introduced into the reaction cell assembly 3 through the gas path assembly 4 to create predetermined gaseous reaction conditions (including vacuum environment) for the solid or liquid sample, and the pressure in the reaction cell assembly 3 is adjusted in real time by adjusting the pressure regulating valve group 5, and when the pressure reaches the predetermined pressure value, the EPR paramagnetic spectrometer 2 is started to scan and detect the sample.

[0049] The detection device can detect a variety of samples, has high universality, and can realize in-situ detection.

[0050] Example two

[0051] The utility model discloses a kind of detection systems, including the in-situ online gas detection device based on electron paramagnetism as example one.

[0052] Obviously, the above examples are only examples for clearly illustrating, and not limit the implementation mode. For ordinary skilled person in the art, other different forms changes or variations can be made on the basis of the above description. Here, it is unnecessary and impossible to exhaust all implementation modes. The obvious changes or variations derived therefrom are still within the protection scope of the utility model.

Claims

1. An in-situ on-line gas detection device based on electron paramagnetism, characterized in that, The utility model relates to an electron paramagnetic resonance (EPR) gas detection device, comprising: a base; an EPR spectrometer arranged on the base, the EPR spectrometer comprising an internal microwave cavity; a reaction cell assembly mounted on the EPR spectrometer, the reaction cell assembly comprising a fixed seat, a bushing, a sample tube and a gas guide tube, the fixed seat having a receiving groove at one end and a gas inlet hole communicating with the receiving groove at the other end, and a gas outlet hole being formed in the side surface of the fixed seat, a plurality of flow guide diffusion holes being formed in the inner wall of the gas outlet hole and communicating with the receiving groove, the bushing being sleeved on the end of the fixed seat provided with the receiving groove, the sample tube being a tube structure with one end sealed, the sealed end of the sample tube extending into the microwave cavity, the open end of the sample tube extending through the bushing into the receiving groove, the gas guide tube being arranged in the sample tube, one end of the gas guide tube being connected with the gas inlet hole and the other end extending to the sealed end of the sample tube; a gas path assembly comprising a reaction tank and a vacuum pump arranged on both sides of the base respectively, the output end of the reaction tank being connected with the gas inlet hole through a gas inlet pipe, and the vacuum pump being connected with the gas outlet hole through a gas outlet pipe.

2. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: A pressure regulating valve is arranged between the reaction tank and the gas inlet pipe.

3. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: Quick connectors are arranged on the gas inlet hole and the gas outlet hole, and the gas inlet pipe and the gas outlet pipe are connected with the gas inlet hole and the gas outlet hole respectively through the quick connectors.

4. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: The base comprises a base body in the shape of a cuboid, the base body being arranged horizontally, and two support frames in the shape of grooves being symmetrically connected to both ends of the base body, the EPR spectrometer being arranged on the base body, and the reaction tank and the vacuum pump being arranged in the two support frames respectively.

5. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: An installation hole communicating with the microwave cavity is formed in the EPR spectrometer, and an installation tube sleeve is coaxially arranged in the installation hole, the sample tube extending through the installation tube sleeve into the microwave cavity.

6. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: The fixed seat is in the shape of a cylinder, a circular groove matching the diameter of the fixed seat being formed in one end of the bushing and the bushing being sleeved on the end of the fixed seat through the circular groove, and a through hole being formed in the bottom of the circular groove, the sample tube extending through the through hole into the receiving groove.

7. The in-situ online gas detection device based on electron paramagnetism according to claim 6, characterized in that: A sealing ring is sleeved on the sample tube and compressed between the fixed seat and the bushing.

8. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: A sealing sleeve is coaxially arranged in the gas inlet hole, and one end of the gas guide tube is sealingly connected with the gas inlet hole through the sealing sleeve.

9. The in-situ online gas detection device based on electron paramagnetism according to claim 1, characterized in that: The sample tube and the gas guide tube are both made of quartz tubes.

10. A detection system characterized by: The utility model relates to an electron paramagnetic resonance (EPR) gas detection device, comprising: any one of claims 1-9.

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