CN116206941A - Anode cooling liquid sampling atmospheric pressure glow discharge ionization device - Google Patents

Anode cooling liquid sampling atmospheric pressure glow discharge ionization device Download PDF

Info

Publication number
CN116206941A
CN116206941A CN202310319011.5A CN202310319011A CN116206941A CN 116206941 A CN116206941 A CN 116206941A CN 202310319011 A CN202310319011 A CN 202310319011A CN 116206941 A CN116206941 A CN 116206941A
Authority
CN
China
Prior art keywords
anode
ionization
component
cavity
cooling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310319011.5A
Other languages
Chinese (zh)
Inventor
郭长娟
宋爽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China Normal University
Original Assignee
South China Normal University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South China Normal University filed Critical South China Normal University
Priority to CN202310319011.5A priority Critical patent/CN116206941A/en
Publication of CN116206941A publication Critical patent/CN116206941A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/025—Detectors specially adapted to particle spectrometers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
    • H01J49/0477—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample using a hot fluid
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to the technical field of chemical component analysis, and discloses an anode cooling liquid sampling atmospheric pressure glow discharge ionization device, which comprises: the ionization source comprises an ionization source cavity, an anode component, a cathode component, a liquid cooling component, an air cooling component and a detection component; the ionization source cavity is provided with an ionization cavity; one end of the anode part is connected with power supply equipment, and the other end penetrates into the ionization cavity; one end of the cathode component is connected with the sample supply equipment and the power supply equipment, and the other end of the cathode component penetrates into the ionization cavity to correspond to the anode component; the cooling areas of the liquid cooling component and the air cooling component correspond to the anode component and are used for cooling the anode component; the detection end of the detection component penetrates into the ionization cavity and corresponds to the reaction areas of the anode component and the cathode component; maintaining the proper temperature of the anode metal can improve the discharge intensity, avoid the problems of poor discharge stability and incapability of ensuring discharge time caused by overhigh discharge environment temperature, and reduce the interference of air interferents on a detection spectrogram; the test safety and reliability are improved.

Description

Anode cooling liquid sampling atmospheric pressure glow discharge ionization device
Technical Field
The invention belongs to the field of chemical spectrum analysis and mass spectrum analysis, and particularly relates to an anode cooling liquid sampling atmospheric pressure glow discharge ionization device.
Background
Heavy metal pollution is becoming more common with the development of the social industry. The pollutants containing heavy metals enter soil, atmosphere and water through various ways to pollute the living environment and endanger the health of human bodies. The soil is polluted by heavy metals, which can cause the yield and quality of crops to be reduced, and can also cause the quality of the atmosphere and the water environment to be further deteriorated. Heavy metals in the atmospheric particulates can enter the human body through the respiratory tract of the human body, thereby affecting the health of the human body. Heavy metal pollutants in the water body can be enriched in the organism, so that the physiological process, the biodiversity and the water body ecological system of the organism are destroyed, and the heavy metal pollutants can enter the human body through a food chain to cause poisoning of the human body. In order to better prevent and treat heavy metal pollution, a detection method for rapidly and accurately detecting heavy metals needs to be established. At present, common heavy metal analysis methods include an inductively coupled plasma mass spectrometry and an inductively coupled plasma atomic emission spectrometry, but the methods have high energy consumption and high cost, and the methods need atomization before sample solution analysis, have large equipment volume, are inconvenient to carry, cannot realize field real-time detection, and can be mostly only used for laboratory detection. Therefore, there is a need to solve these problems, and to achieve real-time, online, and convenient detection of heavy metals to better cope with heavy metal pollution.
In recent years, an atomic emission spectrometer using a liquid sampling glow discharge ionization device as an ionization source is used as a feasible detection means for metal elements in a solution, and gradually enters the field of view of people. When the glow discharge ionization device works, the solution to be measured is input to the top end of the cathode sample injection capillary under the pushing of the peristaltic pump, then the liquid overflows to be contacted with the conductive device, and the conductive device is connected with the negative electrode of the power supply, so that the liquid cathode is formed. The anode metal rod is an ionization source anode, and when a high enough voltage difference is applied between the liquid cathode and the metal anode, glow discharge can be generated between the solution to be detected overflowed from the top end of the cathode sample injection capillary and the anode metal rod. In the glow discharge process, the sample is continuously vaporized, so that metal ions in the vaporized sample enter plasma to be excited to emit characteristic spectrum, and the purpose of detecting metal is achieved. However, most of the current liquid sampling glow discharge ionization devices are used for spectrum analysis, and are used for detecting metal elements, and non-metal elements cannot be detected due to ionization energy and discharge stability. Secondly, during liquid sampling glow discharge spectrum analysis, the discharge temperature is too high along with the increase of discharge time between the metal anode and the liquid cathode, so that the anode metal rod is too high in temperature, the discharge intensity, the discharge stability and the discharge time are affected, and even the anode metal rod is ablated when serious, and the distance between the anode and the cathode is affected. In addition, the liquid sampling glow discharge spectrum is easily affected by discharge environment, such as interference in air, oxygen, hydrogen and water, and the problem of cluttering the spectrogram background can occur.
Disclosure of Invention
The invention aims to provide an anode cooling liquid sampling atmospheric pressure glow discharge ionization device, which solves at least one of the problems in the background art.
In order to solve the technical problems, the specific technical scheme of the invention is as follows:
in some embodiments of the present application, there is provided an anode-cooled liquid sampling atmospheric pressure glow discharge ionization apparatus comprising:
the ionization source cavity is provided with an ionization cavity;
an anode part, one end of which is connected with power supply equipment, and the other end of which penetrates into the ionization cavity;
a cathode part, one end of which is connected with the sample supply device and the power supply device, and the other end of which penetrates into the ionization cavity to correspond to the anode part;
the cooling area of the liquid cooling component corresponds to the anode component and is used for cooling the anode component;
and the detection component is connected with the ionization source cavity, and the detection end of the detection component penetrates into the ionization cavity and corresponds to the reaction areas of the anode component and the cathode component.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the device further comprises an air cooling component, and an air outlet end of the air cooling component penetrates into the ionization cavity to correspond to the anode component.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the detection component is a spectrometer or a mass spectrometer;
when the spectrometer is selected, the anode part and the cathode part are in a 180-degree discharge state;
when a mass spectrometer is selected, the anode part and the cathode part are in a 90 DEG discharge state.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, a first installation opening and a second installation opening which are communicated with the ionization cavity are respectively formed in the top and one side of the ionization source cavity, and the second installation opening corresponds to the detection part; the bottom of the ionization source cavity is provided with a first liquid outlet;
when the anode part is installed in the installation opening, the anode part and the cathode part are in a 180-degree discharge state; the second mounting opening is provided with an observation window;
when the anode part is arranged at the second installation opening, the anode part and the cathode part are in a 90-degree discharge state; and the first mounting opening is provided with an observation window.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the opposite side walls of the first installation opening and the second installation opening are respectively provided with a T-shaped channel I, a T-shaped channel II, a T-shaped channel III and a T-shaped channel IV; the first T-shaped channel and the first T-shaped channel are respectively communicated with the ionization cavity, the outside and the corresponding first mounting opening; the third T-shaped channel and the fourth T-shaped channel are respectively communicated with the ionization cavity, the outside and the corresponding second mounting opening;
when the anode part is arranged at the installation opening, a liquid inlet pipe and a liquid outlet pipe of the liquid cooling part are respectively communicated with a cooling area of the anode part along the first T-shaped channel and the second T-shaped channel, an air outlet pipe of the air cooling part penetrates into the ionization cavity along the third T-shaped channel to correspond to the anode part, and a regulating valve is arranged on the fourth T-shaped channel;
when the anode part is installed at the second installation opening, the liquid inlet pipe and the liquid outlet pipe of the liquid cooling part are respectively communicated with the cooling area of the anode part along the fourth T-shaped channel and the third T-shaped channel, the air outlet pipe of the air cooling part penetrates into the ionization cavity along the second T-shaped channel to correspond to the anode part, and the first T-shaped channel is provided with a regulating valve.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the liquid outlet pipe and the liquid inlet pipe of the liquid cooling component and the air outlet pipe of the air cooling component are fixedly sealed with the corresponding channels through the fixing blocks.
In a preferred embodiment of the above anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the air cooling part comprises:
a gas supply device for supplying a cooling gas;
and the air inlet of the dryer is communicated with the air supply equipment, and the air outlet of the dryer penetrates into the ionization cavity through a pipeline and corresponds to the anode part.
In a preferred embodiment of the above anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the anode part comprises:
an anode conductive block connected to the power supply device,
an anode metal rod, one end of which is connected to the anode conductive block;
the anode fixing assembly is sleeved outside the anode metal rod and is arranged at the first installation opening or the second installation opening; the anode fixing component is provided with a cooling cavity, and the anode metal rod is not in direct contact with the cooling cavity; and the liquid inlet pipe and the liquid outlet pipe of the liquid cooling component are communicated with the cooling cavity.
In a preferred embodiment of the above anode-cooling liquid sampling atmospheric pressure glow discharge ionization device, the cathode member comprises:
one end of the cathode sampling tube penetrates into the ionization cavity and corresponds to the anode metal rod, and the other end of the cathode sampling tube is connected with the sample supply device;
the cathode conductive component is sleeved outside the cathode sampling tube and connected with the power supply equipment;
and the cathode fixing part is sleeved outside the cathode conductive part and is connected with the ionization source cavity.
In the preferable scheme of the anode cooling liquid sampling atmospheric pressure glow discharge ionization device, the device further comprises an ionization source bracket, wherein the ionization source bracket is arranged at the bottom of the ionization source cavity and forms a fixed cavity;
one end of the cathode part is positioned in the fixed cavity, and an electric wire of the power supply equipment is connected with the cathode part through an electric wire hole at one side of the fixed cavity; the liquid supply pipe of the sample supply device penetrates through the ionization source bracket, penetrates through the fixing cavity and is connected with the cathode part; the fixed cavity is provided with a second liquid outlet communicated with the outside.
Compared with the prior art, the invention has the beneficial effects that:
the invention can be used as the ionization source of the spectrometer and the ionization source of the mass spectrometer, can widen the application range of the ionization source and realize the synchronous detection of metal and nonmetal elements;
the liquid cooling component for cooling the anode component is arranged, and the problem of material ablation caused by overhigh anode metal temperature can be avoided by continuously cooling the anode component, so that the requirement of the anode metal material on high-temperature resistance is reduced, and the selection range of the material is improved; the discharge intensity can be improved by keeping the proper temperature of the anode metal, the problems that the discharge stability is poor and the discharge time cannot be ensured due to the fact that the discharge environment temperature is too high are avoided, and the test safety and reliability are improved;
by arranging the air cooling component, the anode component can be subjected to double cooling, and meanwhile, the discharge environment can be purified by utilizing dry cooling gas, so that the interference of air interferents on a detection spectrogram is reduced;
the whole device is simple, portable, flexible and convenient to use and suitable for on-site online real-time detection.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a spectrometer for detection in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a mass spectrometer selected for detection in an embodiment of the present invention.
In the figure:
1. an ionization source cavity; 10. an ionization chamber; 11. a first mounting opening; 12. a second mounting opening; 13. a liquid outlet I; 14. t-shaped channel I; 15. t-shaped channel II; 16. t-shaped channel III; 17. t-shaped channel IV; 2. an anode member; 20. an anode conductive block; 21. an anode metal rod; 220. an anode fixing block I; 221. anode fixed block II; 222. a cooling chamber; 3. a cathode member; 30. a cathode sampling tube; 31. a cathode conductive member; 32. a cathode fixing member; 4. a liquid cooling member; 40. a liquid inlet pipe; 41. a liquid outlet pipe; 42. a cooling water circulator; 50. a spectrometer; 500. a lens fixing barrel; 501. an optical fiber; 502. a condensing lens; 51. a mass spectrometer; 510. an interface fixing block; 511. stainless steel capillary tube; 512. stainless steel capillary sleeve; 6. a sample supply device; 60. a sample liquid supply tube; 7. an ionization source holder; 70. a fixed cavity; 71. a liquid outlet II; 72. an electric wire port; 8. an air-cooling member; 80. an air supply device; 81. a dryer; 82. and cooling the air pipe.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples. The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
In the description of the present application, it should be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate description of the present application and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present application, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art in a specific context.
The present invention will be described in further detail with reference to the accompanying drawings for a better understanding of the objects, structures and functions of the present invention.
Referring to fig. 1-2, an anode-cooled liquid sample atmospheric pressure glow discharge ionization apparatus according to an embodiment of the present application is described, comprising: an ionization source cavity 1, an anode part 2, a cathode part 3, a liquid cooling part 4 and a detection part; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ionization source cavity 1 is provided with an ionization cavity 10; one end of the anode part 2 is connected with power supply equipment, and the other end penetrates into the ionization cavity 10; one end of the cathode part 3 is connected with the sample supply device 6 and the power supply device, and the other end penetrates into the ionization cavity 10 to correspond to the anode part 2; the cooling area of the liquid cooling component 4 corresponds to the anode component 2 and is used for cooling the anode component 2; the detection part is connected to the ionization source cavity 1, and the detection end of the detection part penetrates into the ionization cavity 10 and corresponds to the reaction areas of the anode part 2 and the cathode part 3.
Specifically, the ionization source chamber 1 is preferably made of a solid material having good insulation and thermal conductivity.
The power supply device is a prior art, and may preferably be a glow discharge device. In the process of the electric power device for testing, the power supply equipment supplies power to the anode part 2 and the cathode part 3, so that a high enough voltage difference is formed between the anode part 2 and the cathode part 3, further, glow discharge reaction is realized, in the reaction process, the temperature of the anode part 2 is continuously increased, heat exchange is carried out between cooling water of the liquid cooling part 4 and the anode part 2, heat of the anode part 2 is taken away, and discharge stability can be improved and discharge time can be prolonged.
The sample supply device 6 is preferably a peristaltic pump, and is capable of continuously supplying the sample liquid to the cathode member 3 to form a liquid cathode.
In a preferred version of the above embodiment, the ionization source support 7 is further included, and the ionization source support 7 is disposed at the bottom of the ionization source cavity 1 and forms a fixed cavity 70;
one end of the cathode part 3 is positioned in the fixed cavity 70, and the electric wire of the power supply equipment is connected with the cathode part 3 through the electric wire hole at one side of the fixed cavity 70; the liquid supply pipe of the sample supply device 6 penetrates through the ionization source bracket 7, penetrates through the fixing cavity 70 and is connected with the cathode part 3; the fixed cavity 70 is provided with a second liquid outlet 71 communicated with the outside.
Specifically, the ionization source holder 7 is made of a material with high hardness and good insulation performance, such as polytetrafluoroethylene, ceramic material, etc.
The detecting means is a prior art, and a spectrometer 50 or a mass spectrometer 51 may be used, and a glow discharge device may be used as an ionization source of the spectrometer 50 and the mass spectrometer 51; when the spectrometer 50 is selected, the anode part 2 and the cathode part 3 are in a 180-degree discharge state; when the mass spectrometer 51 is selected, the anode part 2 and the cathode part 3 are in a 90 ° discharge state.
Specifically, a first installation opening 11 and a second installation opening 12 which are communicated with the ionization chamber 10 are respectively formed on the top and one side of the ionization source chamber 1, and the second installation opening 12 corresponds to the detection component; the bottom of the ionization source cavity 1 is provided with a liquid outlet I13;
when the anode part 2 is installed in the first installation opening 11, the anode part 2 and the cathode part 3 are in a 180-degree discharge state; the second mounting opening 12 is provided with an observation window;
when the anode part 2 is arranged in the second mounting opening 12, the anode part 2 and the cathode part 3 are in a 90-degree discharge state; the first mounting opening 11 is provided with a viewing window.
Specifically, the spectrometer 50 interface includes a lens-holding barrel 500, an optical fiber 501, and a condenser lens 502; the mass spectrometer 51 interface includes an interface fixture 510, a stainless steel capillary sleeve 512, and a stainless steel capillary 511; the side wall of the ionization source cavity 1 is provided with a detection opening, which is opposite to the second installation opening 12, when the interface of the spectrometer 50 is selected, the lens fixing barrel 500 is fixed at the detection opening, the optical fiber 501 penetrates along the lens fixing barrel 500, and the condensing lens 502 is installed at the penetrating end of the lens fixing barrel 500; when the interface of the mass spectrometer 51 is selected, the interface fixing block 510 is installed at the detection opening, the stainless steel capillary tube sleeve 512 penetrates into the ionization chamber 10 along the interface fixing block 510, and the stainless steel capillary tube 511 is arranged in the stainless steel capillary tube sleeve 512.
When the spectrometer 50 is selected, the spectrometer 50 is connected with an ionization source through a connection interface of the spectrometer 50, the condensing lens 502 focuses photons in plasma generated by glow discharge, and then a signal is transmitted to the spectrometer 50 through the optical fiber 501 for analysis and detection;
when the mass spectrometer 51 is selected, the mass spectrometer 51 is connected with an ionization source through a mass spectrometer 51 connection interface, and the stainless steel capillary 511 transmits ions in plasma generated by glow discharge to the mass spectrometer 51 for analysis and detection.
Specifically, opposite side walls of the first mounting opening 11 and the second mounting opening 12 are respectively provided with a T-shaped channel I14, a T-shaped channel II 15, a T-shaped channel III 16 and a T-shaped channel IV 17; the T-shaped channel I14 and the T-shaped channel II 15 are respectively communicated with the ionization cavity 10, the outside and the corresponding mounting opening I11; the T-shaped channel III 16 and the T-shaped channel IV 17 are respectively communicated with the ionization chamber 10, the outside and the corresponding mounting opening II 12;
when the anode part 2 is arranged at the first installation opening 11, a liquid inlet pipe 40 and a liquid outlet pipe 41 of the liquid cooling part 4 are respectively communicated with a cooling area of the anode part 2 along a first T-shaped channel 14 and a second T-shaped channel 15, an air outlet pipe of the air cooling part 8 penetrates into the ionization cavity 10 along a third T-shaped channel 16 to correspond to the anode part 2, and a regulating valve is arranged on a fourth T-shaped channel 17 and is used for regulating the pressure intensity of the ionization cavity 10;
when the anode part 2 is installed at the installation opening II 12, the liquid inlet pipe 40 and the liquid outlet pipe 41 of the liquid cooling part 4 are respectively communicated with the cooling area of the anode part 2 along the T-shaped channel IV 17 and the T-shaped channel III 16, the air outlet pipe of the air cooling part 8 penetrates into the ionization cavity 10 along the T-shaped channel II 15 to correspond to the anode part 2, and the T-shaped channel I14 is provided with a regulating valve for regulating the pressure intensity of the ionization cavity 10.
It should be noted that, during the testing process, the pressure in the ionization chamber 10 is too large or too small, and the pressure can be adjusted by the adjusting valve, so as to ensure that the ionization source discharges under the appropriate air pressure condition, and ensure the experimental effect.
Specifically, the liquid cooling member 4 includes a liquid inlet pipe 40, a liquid outlet pipe 41, and a cooling water circulator 42, and when the anode member 2 is mounted in the mounting opening one 11, the liquid inlet pipe 40 and the liquid outlet pipe 41 penetrate into the T-shaped passage one 14 and the T-shaped passage two 15, respectively, from the outside, and communicate with the cooling area of the anode member 2 along the passages; the air outlet pipe of the air cooling part 8 enters along a T-shaped channel III 16 from the outside and is opposite to the anode part 2;
when the anode part 2 is arranged at the second mounting opening 12, the liquid inlet pipe 40 and the liquid outlet pipe 41 respectively penetrate into the T-shaped channel IV 17 and the T-shaped channel III 16 from the outside, and are communicated with the cooling area of the anode part 2 along the channels; the air outlet pipe of the air cooling part 8 enters along the T-shaped channel II 15 from the outside and is opposite to the anode part 2.
Specifically, the liquid outlet pipe 41, the liquid inlet pipe 40 and the liquid outlet pipe are all fixedly sealed with the corresponding channels through fixing blocks.
Specifically, the liquid inlet pipe 40 and the liquid outlet pipe 41 are preferably made of a flexible material having good insulation.
In a preferred version of the above embodiment, the apparatus further comprises an air cooling component 8, and the air outlet end of the air cooling component 8 penetrates into the ionization chamber 10 to correspond to the anode component 2.
Specifically, the air-cooling member 8 includes: a gas supply device 80 and a dryer 81;
the gas supply device 80 is used for supplying cooling gas; the air inlet of the dryer 81 is communicated with the air supply device 80, and the air outlet thereof penetrates into the ionization chamber 10 through the cooling air pipe 82, and corresponds to the anode part 2, and heat of the anode part can be taken away through the cooling air.
It should be noted that, the air supply device 80 and the dryer 81 are both in the prior art, the air supply device 80 may be preferably an air bottle, the compressed cooling gas may be air, helium, argon or the like, and enters the ionization chamber 10 after being dried by the dryer 81, and after the cooled gas flows out, the volume can absorb heat during recovery, and the cooled gas is blown onto the anode component 2 to cool the anode component 2 and purify the surrounding environment, thereby reducing the influence of environmental problems on experimental results.
In a preferred version of the above embodiment, the anode part 2 comprises: an anode conductive block 20, an anode metal rod 21 and an anode fixing assembly;
the anode conductive block 20 is connected to the positive electrode of the power supply device; one end of an anode metal rod 21 is connected with the anode conductive block 20 to form a solid anode; the anode fixing component is sleeved outside the anode metal rod 21 and is arranged at the first mounting opening 11 or the second mounting opening 12; the anode fixing component is provided with a cooling cavity, and the anode metal rod 21 is not in direct contact with the cooling cavity; both the liquid inlet pipe 40 and the liquid outlet pipe 41 of the liquid cooling part 4 are communicated with the cooling cavity 222.
Specifically, the discharge end of the anode metal rod 21 may be pointed or flat.
Specifically, the anode metal rod 21 may be made of a metal material having good heat dissipation properties such as tungsten, molybdenum, copper, or titanium.
Specifically, the diameter of the anode metal rod 21 is preferably 1.0mm, 1.5mm, 2.0mm, 2.5mm or 3.0mm.
Specifically, the anode fixing assembly comprises an anode fixing block one 220 and an anode fixing block two 221, grooves are formed on opposite sides of the anode fixing block one 220 and the anode fixing block two 221, and a cooling cavity 222 is formed after butt joint; the middle parts of the first anode fixing block 220 and the second anode fixing block 221 are respectively provided with a limiting column, one section of the limiting columns is positioned in the cooling cavity 222 after being butted, and the liquid inlet pipe 40 and the liquid outlet pipe 41 are respectively communicated with the cooling cavity 222 to form a cooling circulation pipeline, so that heat generated by the anode metal rod 21 is taken away through water circulation; the limiting cylinder of the anode fixing block II 221 extends into the ionization chamber 10 all the time, and a tubular channel is arranged in the limiting cylinder, so that the anode metal rod 21 can conveniently penetrate from the outside, and the discharge end of the anode metal rod 21 penetrates out of the limiting cylinder and enters the ionization chamber 10.
Specifically, the anode fixing member is preferably made of a material having good heat dissipation.
It should be noted that, the anode conductive block 20 is only electrically connected to the anode metal rod 21, and the anode metal rod 21 is electrically connected to the anode fixing component.
In a preferred version of the above embodiment, the cathode assembly 3 comprises:
a cathode sample tube 30 having one end penetrating into the ionization chamber 10 and corresponding to the anode metal rod 21 and the other end connected to the sample supply device 6 through a sample liquid supply tube 60;
a cathode conductive member 31 which is sleeved outside the cathode sample tube 30 and is connected to a power supply device;
the cathode fixing member 32 is sleeved outside the cathode conductive member 31 and fixed to the ionization source chamber 1.
Specifically, the cathode sampling tube 30 is a cathode sampling capillary tube, and the inner diameter of the cathode sampling capillary tube is preferably 0.2mm, 0.4mm, 0.6mm, 0.8mm or 1.0mm.
Specifically, the cathode conductive member 31 is preferably a cathode conductive tube, and the material is preferably a conductive material such as stainless steel, graphite, or copper.
It should be noted that, the sample rate of the solution to be measured is controlled by the peristaltic pump, and the solution to be measured is input to the top end of the cathode sample tube 30 via the sample hose, the solution to be measured overflows to contact with the cathode conductive tube, and the negative wire of the power supply device penetrates into the fixing cavity 70 via the wire hole 72 and is connected with the cathode conductive member 31, so that the overflowed solution to be measured forms a liquid electrode.
Compared with the prior art, the invention has obvious advantages such as:
the invention can be used as the ionization source of the spectrometer 50 and the ionization source of the mass spectrometer 51, can widen the application range of the ionization source and realize the synchronous detection of metal and nonmetal elements;
the liquid cooling component 4 for cooling the anode component 2 is arranged, and the continuous cooling of the anode component 2 can avoid the problem of material ablation caused by overhigh anode metal temperature, reduce the requirement of anode metal materials on high temperature resistance and improve the selection range of materials; the discharge intensity can be improved by keeping the proper temperature of the anode metal, the problems that the discharge stability is poor and the discharge time cannot be ensured due to the fact that the discharge environment temperature is too high are avoided, and the test safety and reliability are improved;
by arranging the air cooling component 8, the anode component 2 can be optionally cooled down doubly, and the discharge environment can be purified by using dry cooling gas, so that the interference of air interferents on a detection spectrogram is reduced;
the whole device is simple, portable, flexible and convenient to use and suitable for on-site online real-time detection.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. An anode-cooled liquid sampling atmospheric pressure glow discharge ionization device, comprising:
the ionization source cavity is provided with an ionization cavity;
an anode part, one end of which is connected with power supply equipment, and the other end of which penetrates into the ionization cavity;
a cathode part, one end of which is connected with the sample supply device and the power supply device, and the other end of which penetrates into the ionization cavity to correspond to the anode part;
the cooling area of the liquid cooling component corresponds to the anode component and is used for cooling the anode component;
and the detection component is connected with the ionization source cavity, and the detection end of the detection component penetrates into the ionization cavity and corresponds to the reaction areas of the anode component and the cathode component.
2. The anode-cooled liquid sample atmospheric pressure glow discharge ionization device of claim 1, further comprising an air-cooled component, an air-cooled component having an air-out end penetrating into said ionization chamber in correspondence with said anode component.
3. An anode-cooled liquid sampling atmospheric pressure glow discharge ionization apparatus according to claim 1, wherein said detection means is a spectrometer or mass spectrometer;
when the spectrometer is selected, the anode part and the cathode part are in a 180-degree discharge state;
when a mass spectrometer is selected, the anode part and the cathode part are in a 90 DEG discharge state.
4. The anode cooling liquid sampling atmospheric pressure glow discharge ionization device according to claim 3, wherein the top and one side of the ionization source cavity are respectively provided with a first installation opening and a second installation opening which are communicated with the ionization cavity, and the second installation opening corresponds to the detection part; the bottom of the ionization source cavity is provided with a first liquid outlet;
when the anode part is installed in the installation opening, the anode part and the cathode part are in a 180-degree discharge state; the second mounting opening is provided with an observation window;
when the anode part is arranged at the second installation opening, the anode part and the cathode part are in a 90-degree discharge state; and the first mounting opening is provided with an observation window.
5. The anode-cooling liquid sampling atmospheric pressure glow discharge ionization apparatus according to claim 4, wherein said first mounting opening and said second mounting opening have opposite side walls provided with a T-shaped channel one, a T-shaped channel two, a T-shaped channel three and a T-shaped channel four, respectively; the first T-shaped channel and the first T-shaped channel are respectively communicated with the ionization cavity, the outside and the corresponding first mounting opening; the third T-shaped channel and the fourth T-shaped channel are respectively communicated with the ionization cavity, the outside and the corresponding second mounting opening;
when the anode part is arranged at the installation opening, a liquid inlet pipe and a liquid outlet pipe of the liquid cooling part are respectively communicated with a cooling area of the anode part along the first T-shaped channel and the second T-shaped channel, an air outlet pipe of the air cooling part penetrates into the ionization cavity along the third T-shaped channel to correspond to the anode part, and a regulating valve is arranged on the fourth T-shaped channel;
when the anode part is installed at the second installation opening, the liquid inlet pipe and the liquid outlet pipe of the liquid cooling part are respectively communicated with the cooling area of the anode part along the fourth T-shaped channel and the third T-shaped channel, the air outlet pipe of the air cooling part penetrates into the ionization cavity along the second T-shaped channel to correspond to the anode part, and the first T-shaped channel is provided with a regulating valve.
6. The anode cooling liquid sampling atmospheric pressure glow discharge ionization device according to claim 2, wherein the liquid outlet pipe and the liquid inlet pipe of the liquid cooling component and the air outlet pipe of the air cooling component are fixedly sealed with the corresponding channels through the fixing blocks.
7. An anode-cooled liquid sample atmospheric pressure glow discharge ionization apparatus according to claim 2, wherein said air-cooled component comprises:
a gas supply device for supplying a cooling gas;
and the air inlet of the dryer is communicated with the air supply equipment, and the air outlet of the dryer penetrates into the ionization cavity through a pipeline and corresponds to the anode part.
8. An anode-cooled liquid sample atmospheric pressure glow discharge ionization apparatus according to claim 3, wherein said anode means comprises:
an anode conductive block connected to the power supply device,
an anode metal rod, one end of which is connected to the anode conductive block;
the anode fixing assembly is sleeved outside the anode metal rod and is arranged at the first installation opening or the second installation opening; the anode fixing component is provided with a cooling cavity, and the anode metal rod is not in direct contact with the cooling cavity; and the liquid inlet pipe and the liquid outlet pipe of the liquid cooling component are communicated with the cooling cavity.
9. An anode-cooled liquid sample atmospheric pressure glow discharge ionization apparatus according to claim 8, wherein said cathode assembly comprises:
one end of the cathode sampling tube penetrates into the ionization cavity and corresponds to the anode metal rod, and the other end of the cathode sampling tube is connected with the sample supply device;
the cathode conductive component is sleeved outside the cathode sampling tube and connected with the power supply equipment;
and the cathode fixing part is sleeved outside the cathode conductive part and is connected with the ionization source cavity.
10. The anode-cooled liquid sampling atmospheric pressure glow discharge ionization device of claim 1, further comprising an ionization source holder disposed at the bottom of said ionization source cavity and forming a stationary cavity;
one end of the cathode part is positioned in the fixed cavity, and an electric wire of the power supply equipment is connected with the cathode part through an electric wire hole at one side of the fixed cavity; the liquid supply pipe of the sample supply device penetrates through the ionization source bracket, penetrates through the fixing cavity and is connected with the cathode part; the fixed cavity is provided with a second liquid outlet communicated with the outside.
CN202310319011.5A 2023-03-28 2023-03-28 Anode cooling liquid sampling atmospheric pressure glow discharge ionization device Pending CN116206941A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310319011.5A CN116206941A (en) 2023-03-28 2023-03-28 Anode cooling liquid sampling atmospheric pressure glow discharge ionization device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310319011.5A CN116206941A (en) 2023-03-28 2023-03-28 Anode cooling liquid sampling atmospheric pressure glow discharge ionization device

Publications (1)

Publication Number Publication Date
CN116206941A true CN116206941A (en) 2023-06-02

Family

ID=86507757

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310319011.5A Pending CN116206941A (en) 2023-03-28 2023-03-28 Anode cooling liquid sampling atmospheric pressure glow discharge ionization device

Country Status (1)

Country Link
CN (1) CN116206941A (en)

Similar Documents

Publication Publication Date Title
US10705023B2 (en) Solution cathode glow discharge plasma-atomic emission spectrum apparatus and method capable of performing direct gas sample introduction and used for detecting heavy metal element
He et al. Flowing and nonflowing liquid electrode discharge microplasma for metal ion detection by optical emission spectrometry
CN105185686B (en) Ion mobility spectrometry employing electrospray/corona discharge dual-mode ion source
CN103163116A (en) Liquid cathode glow discharge emission spectrum detection metal ion apparatus
CN106568833B (en) A kind of liquid cathode glow discharge optical emission spectrometry device and method for heavy metal analysis
CN106596515B (en) Pulse voltage drive-type arc discharge plasma source and Portable element spectrometer
CA2556558A1 (en) Analytical method and analyzer capable of substantially simultaneously analyzing absorption/emission/scattering spectrum and mass spectrum, and analytical method and mass spectroscope utilizing electrospray ionization technique
CN102271451B (en) A kind of cathode construction of laminar flow electric arc plasma generator
US20130009055A1 (en) System of electrospray ion generator
CN103776818A (en) Glow discharge-based plasma generator and spectrum detection system formed by same
CN103887142A (en) Discharge photoionization source in linear acceleration type flight time mass spectrum
CN103236394A (en) Microwave plasma based atmospheric pressure desorption ion source and application thereof
WO2005024387A3 (en) Capillary-discharge based detector for chemical vapor monitoring
CN116206941A (en) Anode cooling liquid sampling atmospheric pressure glow discharge ionization device
US8642917B2 (en) Highly ordered structure pyrolitic graphite or carbon-carbon composite cathodes for plasma generation in carbon containing gases
CN203658269U (en) Plasma exciting spectrum detection system based on glow discharge
CN105651760B (en) A kind of microplasma device of the metallic element analysis suitable for gas
CN110828282B (en) Ion source device for liquid chromatogram and ion mobility spectrometry and application
CN211376584U (en) Heating capillary liquid cathode glow discharge ionization device
Zhu et al. Determination of nitrate and ammonium ions in water samples by atmospheric pressure glow discharge microplasma molecular emission spectrometry coupled with chemical vapour generation
CN211237475U (en) Direct current glow discharge probe diagnostic device for teaching
CN212844962U (en) Excitation source device of heavy metal detector
CN111935894A (en) Atmospheric pressure liquid anode glow discharge plasma device
CN109187496B (en) Atomic emission spectrum analysis device based on electrothermal evaporation and tip discharge
CN216015292U (en) High-sample-utilization-rate ion source device for mass spectrometer

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination