CN111929290A - Atomic emission spectrum device of tungsten filament electric heating evaporation-atmospheric pressure glow discharge - Google Patents
Atomic emission spectrum device of tungsten filament electric heating evaporation-atmospheric pressure glow discharge Download PDFInfo
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- 238000001636 atomic emission spectroscopy Methods 0.000 claims abstract description 11
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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Abstract
The atomic emission spectroscopy device of tungsten filament electrothermal evaporation-atmospheric pressure glow discharge of the invention, possess: the device comprises an atmospheric pressure glow discharge device, a cathode stainless steel tube, a coaxial quartz tube, a beam quartz tube, an anode tungsten tube, a cathode stainless steel tube, a beam quartz tube, an anode tungsten tube, a cathode stainless steel tube, an anode tungsten tube, a coaxial quartz tube, a beam quartz tube, a cathode stainless steel tube, an anode tungsten tube, a cathode stainless steel tube, an anode; the tungsten filament electrothermal evaporation/atomizer comprises a transmission tube, a tungsten filament coil, a power supply base, a lead and a quartz cover, wherein the quartz cover is provided with a carrier gas inlet, a carrier gas outlet and a sample inlet; and a detection system. The invention can improve the detection capability of heavy metal elements.
Description
Technical Field
The invention belongs to the field of atomic spectrum analysis, relates to the technical field of atomic emission spectrum excitation sources, and more particularly relates to a tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectrum device which can be applied to the field of atomic emission spectrum.
Background
Atmospheric Pressure Glow Discharge (APGD) is a plasma with a size limited to millimeter or even lower, and has the advantages of Atmospheric Pressure operation, simple structure, low power consumption and the like, and has the potential of miniaturization and portability, so that the APGD is widely concerned by students in the field of spectral mass spectrometry and is increasingly applied to atomic spectral mass spectrometry research. However, the excitation temperature of the APGD microplasma region is low, and the excitation capability of the APGD microplasma region to some heavy metal elements with high excitation energy is not sufficient, so that the APGD microplasma region has low sensitivity to the elements and high detection limit. In addition, studies have shown that moisture has a major impact on both the excitability and stability of APGD. Therefore, it is desirable to improve the analytical sensitivity, stability and analytical application range of APGD using a sample injection method that can improve microplasma excitation capability without introducing excessive moisture.
Electrothermal Evaporation (ETV) is a sample introduction technique that introduces minute amounts of liquid (or solid) samples into a plasma in a pulsed manner. Specifically, microliter or milligram samples are deposited in a metal or graphite material vaporizer and the dry aerosol generated by resistive heating is introduced into the plasma via a carrier gas for analysis. The sample is converted into a gaseous form through electrothermal evaporation and is introduced into the excitation unit, so that the sample injection efficiency is higher; secondly, the desolventizing, matrix removing, evaporating and atomizing of the sample are completed in an independent electric heating component, so that the influence of moisture and matrix in the sample on the energy consumption and stability of the excitation unit is effectively reduced, the excitation capability is improved, and the detection sensitivity is improved. Tungsten filament (W-coil) as a high temperature resistant device capable of resisting high temperature above 2000 deg.C has the advantages of small volume, low price, low power consumption, fast temperature rise rate, etc., and is widely used in atomic spectrum electric heating evaporation sample introduction method as an electric heating evaporation device.
Disclosure of Invention
In view of this, the present invention aims to provide a tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy apparatus, which can effectively remove moisture and matrix in a sample, improve APGD excitation capability and stability, and improve detection capability of heavy metal elements.
The invention relates to a tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectrum device, which comprises:
an atmospheric pressure glow discharge device;
a tungsten filament electrothermal evaporation/atomizer for inputting carrier gas and a sample to be analyzed into the atmospheric pressure glow discharge device;
a detection system for receiving the atomic emission spectrum signal generated by the atmospheric pressure glow discharge device;
a power supply system for supplying electrical energy;
the atmospheric pressure glow discharge device includes: the beam current quartz tube and the anode tungsten tube are fixed into a whole by the coaxial quartz tube, the cathode stainless steel tube and the anode tungsten tube are kept coaxial, and the coaxial quartz tube and the beam current quartz tube are arranged in the outer quartz tube;
the tungsten filament electrothermal evaporation/atomizer comprises: the device comprises a transmission pipe, a tungsten wire coil, a power supply base, a lead and a quartz cover, wherein the quartz cover is provided with a carrier gas inlet, a carrier gas outlet and a sample inlet, the carrier gas inlet is connected with a gas flow controller and a carrier gas bottle, the carrier gas outlet is coaxially connected with the cathode stainless steel pipe of the atmospheric pressure glow discharge device through the transmission pipe, the tungsten wire coil is installed on the power supply base and is arranged in the quartz cover together, and the power supply base is connected to a power supply system through the lead.
According to the invention, the atomic emission spectrometry device with the tungsten filament electrothermal evaporation/atomizer and the APGD connected in series can be realized, and the advantages of the tungsten filament electrothermal evaporation/atomizer and the APGD are fully exerted. Specifically, the cathode stainless steel tube is embedded in the beam quartz tube, so that the effective volume of glow discharge is limited, and the discharge energy density is improved. The coaxial nested design of the atmospheric pressure glow discharge device ensures that the atmospheric pressure glow discharge device has higher integration level, improves the discharge energy density of APGD, and allows the acquisition of spectral signals along the axial direction of the atmospheric pressure glow discharge device by ensuring that the cathode and the anode are coaxial. The tungsten filament electrothermal evaporation/atomization device can quickly enter dry aerosol containing the analyte into APGD for further excitation after completing drying, pyrolysis, evaporation/atomization of a test, and the condensation loss in a pipeline is reduced.
In the invention, the detection system may include a computer and a spectrometer connected to the computer, and a fiber probe of the spectrometer is aligned to one end of the anode tungsten tube along an axial direction of the atmospheric pressure glow discharge device.
According to the invention, only the anode tungsten tube needs to be aligned, and the light path does not need to be carefully adjusted, so that the debugging time of the device and the experimental stability are saved.
In the present invention, an ultraviolet fused silica plane window may be disposed between the atmospheric pressure glow discharge device and the optical fiber probe.
According to the invention, the ultraviolet fused quartz plane window can isolate the high-temperature afterglow blown out from the anode tungsten tube, and plays a role in protecting the optical fiber probe.
In the invention, the quartz cover is a three-way structure with a carrier gas inlet, a carrier gas outlet and a sample inlet, and the main body is a quartz tube with the height of 42-45mm, the outer diameter of 21-22mm and the inner diameter of 18 mm; the sample inlet, the carrier gas inlet and the carrier gas outlet are respectively fine quartz tubes with the inner diameters of 2-6mm, 2-3mm and 2-3mm, and are respectively fired at the position 23-25mm away from the bottom of the front surface of the main body, and the position 8-12mm away from the bottom and the top of the side surface of the main body.
According to the invention, the device is very small and convenient to be used together with an APGD device.
In the invention, the conveying pipe can be a silica gel hose with the length of 40mm-60 mm.
According to the invention, the transmission pipe is used for connecting the ETV and the APGD transmission samples, and the shorter the transmission pipe distance is, the less the samples are lost on the transmission path.
In the present invention, the carrier gas cylinder may transport H2-He mixed gas as discharge medium of atmospheric pressure glow discharge and sample transmissionAnd (4) conveying the carrier gas.
According to the invention, H is used2The mixed gas of-He is used as a discharge medium between a cathode stainless steel tube and an anode tungsten tube in the atmospheric pressure glow discharge device, uniform and stable microplasma is generated, and dry aerosol containing the analyte in the tungsten filament electrothermal evaporation/atomizer is sent to the atmospheric pressure glow discharge device for excitation. H in the gas mixture2Partial stray light in an atomic emission spectrum emitted by the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic spectrum device can be eliminated, so that the spectrum can be used for detection and analysis. In addition H2Reducing atmosphere can be formed, oxidation loss caused by high-temperature evaporation of the tungsten wire coil is reduced, and the service life is prolonged.
In the present invention, the H may be23% -10% of H in mixed gas of-He2，90-97%He。
According to the present invention, a spectrum signal due to air impurities can be partially eliminated after adding hydrogen gas to helium gas, so that the spectrum can be used for actual sample analysis. In addition, hydrogen can provide reducing atmosphere, oxidation of the tungsten filament at a high temperature is reduced, and the service life of the tungsten filament is prolonged.
In the present invention, the atmospheric pressure glow discharge device may be disposed in the T-shaped three-way valve; the device also comprises a fixing pipe for fixing the atmospheric pressure glow discharge device in the T-shaped three-way valve.
According to the invention, the atmospheric pressure glow discharge device can be fixed by adopting a T-shaped three-way valve, and the purpose of fixing the atmospheric pressure glow discharge device in the T-shaped three-way valve by using the fixing pipe is to ensure that the whole device is easily fixed on a three-dimensional platform and kept horizontal. Specifically, the outer diameter of the outer quartz tube in the coaxial nested structure of the APGD is consistent with the inner diameter of the three-way valve and can be directly inserted into the outer diameter of the outer quartz tube, but the outer diameter of the inner beam quartz tube is smaller than the inner diameter of the three-way valve and can be fixed in the three-way valve only by being inserted into the fixing tube.
The invention also can comprise a rubber tube and a clamp for sealing the sample inlet.
The use of this sealing means is more convenient than the use of a sealing plug according to the invention.
In the present invention, the power supply system may include two dc power supplies for supplying power to the atmospheric pressure glow discharge device and the tungsten filament electrothermal evaporation/atomizer, respectively.
According to the invention, two direct current power supplies with different powers can be used for respectively providing electric energy for the atmospheric glow discharge device and the tungsten filament electrothermal evaporation/atomizer.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device according to an embodiment of the present invention;
FIG. 2 is an atomic emission spectrum of an exemplary application of the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy apparatus of the present invention to Cd element;
reference numerals:
1-gas carrying bottle 2-gas flow controller 3-tungsten wire coil 4-power base 5-quartz cover 6-carrier gas inlet 7-carrier gas outlet 8-sample inlet 9-rubber tube 10-clamp 11-transmission tube 12-T type three-way valve 13-fixed tube 14-outer side quartz tube 15-coaxial quartz tube 16-beam quartz tube 17-cathode stainless steel tube 18-anode tungsten tube 19-ultraviolet fused quartz plane window 20-optical fiber probe 21-spectrometer 22-computer 23-power supply 24-resistor 25-heating power supply 26-resistor 27-wire.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting thereof.
Fig. 1 is a schematic diagram of the overall structure of a tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device according to an embodiment of the present invention. As shown in fig. 1, the atomic emission spectroscopy apparatus of tungsten filament electrothermal evaporation-atmospheric glow discharge according to the present embodiment includes: a T-shaped three-way valve 12; an atmospheric glow discharge device provided on the T-shaped three-way valve 12; a tungsten filament electrothermal evaporation/atomizer which inputs carrier gas and a sample to be analyzed into the atmospheric pressure glow discharge device and is communicated with the T-shaped three-way valve 12; a detection system for receiving atomic emission spectrum signals generated by the atmospheric pressure glow discharge device; and the power supply system provides electric energy for the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectrometry device.
As shown in fig. 1, in the atomic emission spectroscopy device of tungsten filament electrothermal evaporation-atmospheric pressure glow discharge according to the present embodiment, the atmospheric pressure glow discharge device includes an outer quartz tube 14, a beam quartz tube 16, a coaxial quartz tube 15, a cathode stainless steel tube 17, and an anode tungsten tube 18. The anode tungsten tube 18 is an anode hollow tungsten tube.
Specifically, in the above atmospheric pressure glow discharge device, the cathode stainless steel tube 17 is embedded in the beam quartz tube 16 having a matched size, and the outer wall of the cathode stainless steel tube 17 is attached to the inner wall of the beam quartz tube 16. By means of the method, the cathode stainless steel tube is embedded in the beam quartz tube with the matched size, the effective volume of glow discharge is limited, and the discharge energy density is improved.
In the atmospheric glow discharge device, a beam quartz tube 16 having a cathode stainless steel tube 17 embedded therein and an anode tungsten tube 18 are fixed together by a coaxial quartz tube 15, and the cathode stainless steel tube 17 and the anode tungsten tube 18 are kept coaxial. And a fixed coaxial quartz tube-beam quartz tube which is internally embedded with a cathode stainless steel tube 17 and an anode tungsten tube 18 is arranged in the outer quartz tube 14.
According to the invention, the coaxial nested design of the atmospheric pressure glow discharge device ensures that the atmospheric pressure glow discharge device has higher integration level, improves the discharge energy density of APGD, and allows the acquisition of the spectrum signal along the axial direction of the atmospheric pressure glow discharge device by ensuring that the cathode and the anode are coaxial.
In addition, the atomic emission spectroscopy device of tungsten filament electrothermal evaporation-atmospheric pressure glow discharge of the present embodiment further includes a fixing tube 13 for fixing the atmospheric pressure glow discharge device in the T-shaped three-way valve 12. The specific fixing method can be, for example, inserting one end of a beam quartz tube into a fixed tube, and then placing the fixed tube in a right one-way in a T-shaped three-way valve. The outer quartz tube is inserted into the left through hole of the T-shaped three-way valve. The reason for using the T-shaped three-way valve is that a cooling gas can be introduced from the top of the T-shaped three-way valve, but the T-shaped three-way valve is not required to be used in the present embodiment and only serves the purpose of fixing the atmospheric glow discharge device. Preferably, the T-shaped three-way valve 12 is a stainless steel T-shaped three-way valve. The fixed pipe 13 may be made of, for example, polytetrafluoroethylene.
As shown in fig. 1, in the atomic emission spectroscopy apparatus of tungsten filament electrothermal evaporation-atmospheric pressure glow discharge according to the present embodiment, the tungsten filament electrothermal evaporation/atomizer includes a transmission tube 11, a tungsten filament coil 3, a power base 4, a lead 27, and a quartz cover 5, the quartz cover 5 includes a carrier gas inlet 6, a carrier gas outlet 7, and a sample inlet 8, and the carrier gas inlet 6 is connected to a gas flow rate controller 2 and a gas carrying bottle 1. The carrier gas cylinder 1 may be, for example, a carrier gas cylinder. The power base 4 is connected to the power system via a wire 27.
Specifically, the tungsten coil 3 is mounted on the power base 4 and inserted together into the quartz capsule 5.
Preferably, in the electrothermal evaporation/atomizer of the tungsten filament according to the present embodiment, the quartz cap 5 has a three-way structure, and the main body is a quartz tube having a height of 45mm, an outer diameter of 21 mm, and an inner diameter of 18 mm. The sample inlet, the carrier gas inlet and the carrier gas outlet are respectively fine quartz tubes with the inner diameters of 6mm, 3mm and 2mm, the fine quartz tubes are respectively fired at the position 25mm away from the bottom of the front face of the main quartz tube, and the position 10 mm away from the bottom and the top of the side face of the main quartz tube. In the embodiment shown in fig. 1, the quartz cover 5 has a bottom portion at the end closer to the power base 4 and a top portion at the end opposite to the power base 4.
Preferably, a rubber tube 9 and a clamp 10 for sealing the sample inlet 8 are also included. The clamp 10 may be, for example, a binder clip.
In addition, the carrier gas outlet 7 of the tungsten filament electrothermal evaporation/atomizer of the embodiment is connected with a cathode stainless steel tube 17 of an atmospheric pressure glow discharge device through a transmission tube 11, and the transmission tube 11 can be a silica gel hose with the length of 40mm-60 mm.
By means of the device, the tungsten filament electrothermal evaporation/atomization device can quickly enter the APGD to be further excited after drying, pyrolysis, evaporation/atomization of a test, and condensation loss in a pipeline is reduced.
Preferably, in the present embodiment, the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device uses H2-He (e.g. 3% H)297% He) gas mixture as the discharge medium for atmospheric pressure glow discharge and the sample transport carrier gas.
With the aid of this, H2The mixed gas of-He is used as a discharge medium between a cathode stainless steel tube and an anode tungsten tube in the atmospheric pressure glow discharge device, uniform and stable microplasma is generated, and dry aerosol containing the analyte in the tungsten filament electrothermal evaporation/atomizer is sent to the atmospheric pressure glow discharge device for excitation. H in the gas mixture2Partial stray light in an atomic emission spectrum emitted by the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic spectrum device can be eliminated, so that the spectrum can be used for detection and analysis. In addition H2Reducing atmosphere can be formed, oxidation loss caused by high-temperature evaporation of the tungsten wire coil is reduced, and the service life is prolonged.
As shown in fig. 1, the power supply system for supplying electric energy to the tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device can respectively supply electric energy to the atmospheric pressure glow discharge device and the tungsten filament electrothermal evaporation/atomizer by two direct current power supplies with different powers. Such as the high voltage power supply 23 shown in fig. 1 for powering an atmospheric glow discharge device and the heating power supply 25 for powering an electrothermal evaporation/atomizer of tungsten filaments. And a resistor 24 of 10 k omega, 225W is connected in series in the atmospheric pressure glow discharge device, and a resistor 26 of 2.5 omega, 1000W is connected in series in the tungsten filament electrothermal evaporation/atomizer.
Therefore, the series resistor can prevent the APGD from being converted into electric arc in the process of generating the microplasma, and the stability of the APGD microplasma is improved. In addition, because the resistance of the tungsten wire coil is extremely small, the high-power resistance can prevent short circuit and play a role in protecting a direct-current power supply.
In addition, the detection system of the atomic emission spectrum signal generated by the atmospheric pressure glow discharge device is characterized in that an optical fiber probe 20 of a spectrometer 21 connected with a computer 22 is axially arranged along the atmospheric pressure glow discharge device, and an ultraviolet fused quartz plane window 19 is arranged between the atmospheric pressure glow discharge device and the optical fiber probe 20.
With this, the ultraviolet fused silica flat window 19 can isolate the high-temperature afterglow blown out from the anode tungsten tube 18, and plays a role of protecting the optical fiber probe 20.
The operation flow of the invention is exemplified as follows:
1) 10 mu L of sample is dripped on the tungsten wire coil 3 through the sample inlet 8, and the rubber tube 9 sleeved on the sample inlet is folded in half and then clamped and sealed by the long tail clamp 10.
2) And opening the carrier gas steel cylinder 1 and the gas flow controller 2, introducing carrier gas, controlling a heating power supply 25 externally connected with the tungsten filament electrothermal evaporation/atomization device to carry out temperature programming, and starting drying, substrate removal, cooling, preheating, evaporation/atomization on the sample. Specifically, these steps can be realized by operating a supporting program on a computer, for example, setting the current magnitude of the heating power supply and the holding time at the current, and completing the heating after the tungsten wire is heated.
3) And (3) in the cooling stage in the step (2), turning on a high-voltage power supply 23 externally connected to the atmospheric pressure glow discharge device, and finishing ignition through a conductive metal wire to generate uniform and stable microplasma. The conductive wire is a separate component that is used only when ignited, such as a disposable medical syringe. The principle and process of ignition are that after carrier gas is introduced into the cathode stainless steel tube and the anode tungsten tube and electric conduction is carried out, a loop can be formed only after the electrodes are contacted. However, the error is increased by moving the electrode during each sample injection, so that the electrode is fixed, the needle of the injector is inserted from the anode port, the needle is positively charged at the moment, the discharge is generated when the needle approaches the cathode, the needle is withdrawn from the anode port at the moment, and the discharge is extended to the anode tube, so that the ignition process is completed. Thus, the syringe needle may be replaced with other electrically conductive wire-like materials.
4) After the preheating and evaporation/atomization processes in the step (2), the sample on the tungsten wire coil 3 is changed into a dry aerosol form and is transmitted to an atmospheric pressure glow discharge device through carrier gas for excitation, a characteristic atomic emission spectrum is generated, the sample is received by the optical fiber probe 20 through the ultraviolet fused quartz plane window 19, and the sample is detected by the spectrometer 21.
5) After the signal collection is finished, the tungsten wire coil 3 is heated again for cleaning, and the next sample introduction can be carried out after cooling.
Fig. 2 is a graph of net signal intensity at multiple wavelengths for cadmium detected using the above-described apparatus.
As the present invention may be embodied in several forms without departing from the spirit of essential characteristics thereof, the present embodiments are therefore illustrative and not restrictive, since the scope of the invention is defined by the appended claims rather than by the description herein, and all changes that fall within metes and bounds of the claims, or equivalence of such metes and bounds thereof are therefore intended to be embraced by the appended claims.
Claims (10)
1. An atomic emission spectroscopy device of tungsten filament electrothermal evaporation-atmospheric pressure glow discharge is characterized by comprising:
an atmospheric pressure glow discharge device;
a tungsten filament electrothermal evaporation/atomizer for inputting carrier gas and a sample to be analyzed into the atmospheric pressure glow discharge device;
a detection system for receiving the atomic emission spectrum signal generated by the atmospheric pressure glow discharge device;
a power supply system for supplying electrical energy;
the atmospheric pressure glow discharge device includes: the beam current quartz tube and the anode tungsten tube are fixed into a whole by the coaxial quartz tube, the cathode stainless steel tube and the anode tungsten tube are kept coaxial, and the coaxial quartz tube and the beam current quartz tube are arranged in the outer quartz tube;
the tungsten filament electrothermal evaporation/atomizer comprises: the device comprises a transmission pipe, a tungsten wire coil, a power supply base, a lead and a quartz cover, wherein the quartz cover is provided with a carrier gas inlet, a carrier gas outlet and a sample inlet, the carrier gas inlet is connected with a gas flow controller and a carrier gas bottle, the carrier gas outlet is coaxially connected with the cathode stainless steel pipe of the atmospheric pressure glow discharge device through the transmission pipe, the tungsten wire coil is installed on the power supply base and is arranged in the quartz cover together, and the power supply base is connected to a power supply system through the lead.
2. The atomic emission spectroscopy device for tungsten filament electrothermal evaporation-atmospheric pressure glow discharge according to claim 1, wherein the detection system comprises a computer and a spectrometer connected with the computer, and a fiber probe of the spectrometer is aligned with one end of the anode tungsten tube along the axial direction of the atmospheric pressure glow discharge device.
3. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device of claim 2, wherein an ultraviolet fused quartz planar window is placed between the atmospheric pressure glow discharge device and the fiber probe.
4. The atomic emission spectroscopy device of electrothermal evaporation of tungsten filament-atmospheric pressure glow discharge of claim 1, wherein the main body of the quartz cover is a quartz tube with a height of 42-45mm, an outer diameter of 21-22mm and an inner diameter of 18 mm; the sample inlet, the carrier gas inlet and the carrier gas outlet are respectively fine quartz tubes with the inner diameters of 2-6mm, 2-3mm and 2-3mm, and are respectively fired at the position 23-25mm away from the bottom of the front surface of the main body, and the position 8-12mm away from the bottom and the top of the side surface of the main body.
5. The atomic emission spectroscopy device of electrothermal evaporation of tungsten filament-atmospheric pressure glow discharge of claim 1, wherein the transmission tube is a silica gel hose with a length of 40mm-60 mm.
6. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device of claim 1, wherein the carrier gas cylinder delivers H2The mixed gas of-He is used as a discharge medium of the atmospheric pressure glow discharge and a sample transmission carrier gas.
7. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device of claim 6, wherein the H is23% -10% of H in mixed gas of-He2，90-97%He。
8. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device of claim 1, wherein the atmospheric pressure glow discharge device is arranged on a T-shaped three-way valve; the device also comprises a fixing pipe for fixing the atmospheric pressure glow discharge device in the T-shaped three-way valve.
9. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device according to claim 1, further comprising a rubber tube and a clamp for sealing the sample inlet.
10. The tungsten filament electrothermal evaporation-atmospheric pressure glow discharge atomic emission spectroscopy device of claim 1, wherein the power supply system comprises two direct current power supplies for respectively supplying power to the atmospheric pressure glow discharge device and the tungsten filament electrothermal evaporation/atomizer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113630950A (en) * | 2021-07-28 | 2021-11-09 | 中国地质大学（武汉） | Liquid anode glow discharge micro-plasma excitation source and excitation method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5549046A (en) * | 1994-05-05 | 1996-08-27 | General Dynamics Land Systems, Inc. | Plasma generator for electrothermal gun cartridge |
| CN1476284A (en) * | 2002-07-02 | 2004-02-18 | ��־�������ʽ���� | Lighting device for high-pressure discharge lamp |
| US20110234102A1 (en) * | 2008-11-26 | 2011-09-29 | Ik Nyeon Kim | Apparatus for normal pressure plasma ignition and method for normal pressure plasma ignition using same |
| CN203534972U (en) * | 2013-11-12 | 2014-04-09 | 四川大学 | Atomic emission spectrum analysis device based on electric heating evaporation-dielectric barrier discharge |
| CN105717055A (en) * | 2016-03-11 | 2016-06-29 | 中国农业科学院农业质量标准与检测技术研究所 | Device and method for measuring zinc through electric heating evaporation atomic absorption spectrometry method |
| CN106290210A (en) * | 2016-08-04 | 2017-01-04 | 中国地质大学（武汉） | The method of a kind of atmospheric pressure glow discharge detection metal ion and detecting system |
| CN107991272A (en) * | 2017-11-24 | 2018-05-04 | 中国地质大学（武汉） | A kind of portable atmospheric pressure glow discharge microplasma spectrometer and its implementation |
| US20180372646A1 (en) * | 2015-12-31 | 2018-12-27 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | 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 |
-
2019
- 2019-05-13 CN CN201910394036.5A patent/CN111929290A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5549046A (en) * | 1994-05-05 | 1996-08-27 | General Dynamics Land Systems, Inc. | Plasma generator for electrothermal gun cartridge |
| CN1476284A (en) * | 2002-07-02 | 2004-02-18 | ��־�������ʽ���� | Lighting device for high-pressure discharge lamp |
| US20110234102A1 (en) * | 2008-11-26 | 2011-09-29 | Ik Nyeon Kim | Apparatus for normal pressure plasma ignition and method for normal pressure plasma ignition using same |
| CN203534972U (en) * | 2013-11-12 | 2014-04-09 | 四川大学 | Atomic emission spectrum analysis device based on electric heating evaporation-dielectric barrier discharge |
| US20180372646A1 (en) * | 2015-12-31 | 2018-12-27 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | 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 |
| CN105717055A (en) * | 2016-03-11 | 2016-06-29 | 中国农业科学院农业质量标准与检测技术研究所 | Device and method for measuring zinc through electric heating evaporation atomic absorption spectrometry method |
| CN106290210A (en) * | 2016-08-04 | 2017-01-04 | 中国地质大学（武汉） | The method of a kind of atmospheric pressure glow discharge detection metal ion and detecting system |
| CN107991272A (en) * | 2017-11-24 | 2018-05-04 | 中国地质大学（武汉） | A kind of portable atmospheric pressure glow discharge microplasma spectrometer and its implementation |
Non-Patent Citations (4)
| Title |
|---|
| 彭晓旭: "He气氛大气压辉光放电原子发射光谱装置的构建及其增敏研究", 《第五届全国原子光谱及相关技术学术会议摘要集》 * |
| 彭晓旭: "He气氛大气压辉光放电原子发射光谱装置的构建及其增敏研究", 《第五届全国原子光谱及相关技术学术会议摘要集》, 23 September 2018 (2018-09-23), pages 0002 * |
| 汤志勇等: "原子发射光谱分析", 《分析试验室》 * |
| 汤志勇等: "原子发射光谱分析", 《分析试验室》, no. 12, 30 December 2011 (2011-12-30) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113630950A (en) * | 2021-07-28 | 2021-11-09 | 中国地质大学（武汉） | Liquid anode glow discharge micro-plasma excitation source and excitation method |
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