CN211318204U - On-line detection device for sodium aerosol in air - Google Patents

On-line detection device for sodium aerosol in air Download PDF

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CN211318204U
CN211318204U CN201921087733.8U CN201921087733U CN211318204U CN 211318204 U CN211318204 U CN 211318204U CN 201921087733 U CN201921087733 U CN 201921087733U CN 211318204 U CN211318204 U CN 211318204U
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atomic emission
spectrum
sodium
line detection
detection device
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杜海鸥
周培德
段忆翔
朴君
申凤阳
谢淳
王荣东
王国芝
石文涛
韩新梅
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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Abstract

The disclosure belongs to the technical field of reactors, and particularly relates to an online detection device for sodium aerosol in reactor air. The device includes: the device comprises a sampling and shunting device, an atomic emission spectrum excitation source, a spectrum monitoring device and a correction bottle; wherein the sampling shunt device delivers the air sample to the atomic emission spectroscopy excitation source; the atomic emission spectrum excitation source excites sodium aerosol in an air sample to form an atomic emission spectrum, and the atomic emission spectrum is collected through a spectrum monitoring device; the spectrum monitoring device separates the emitted light of the sodium atoms and converts the light into an electric signal; the calibration vial provides an aerosol sample of known concentration to an atomic emission spectroscopy excitation source. Therefore, the on-line detection device for the sodium aerosol in the air, which has long-term stable operation, low energy consumption and low detection limit, is provided.

Description

On-line detection device for sodium aerosol in air
Technical Field
The disclosure belongs to the technical field of reactors, and particularly relates to an online detection device for sodium aerosol in reactor air.
Background
The fast neutron reactor uses liquid metal sodium as a coolant. The high-temperature sodium in the container and the pipeline can not be burnt in contact with air under normal conditions. When an accident occurs to cause the damage of a pipeline or equipment, high-temperature liquid sodium is likely to leak into the air to be combusted, the sodium combustion can cause serious damage to the equipment and room structures, and simultaneously, a large amount of harmful sodium aerosol is generated. Therefore, how to realize early accurate detection of sodium leakage is one of key problems needing key breakthrough and solution in sodium fire detection, so as to provide more important guarantee for fast reactor safety.
The devices currently used for the detection of sodium aerosols in the air comprise: smoke detectors, sodium ionization detectors, differential pressure detectors, flame furnace atomization detectors, laser detectors, and the like. The smoke detector is used as a conventional fire detector, responds to all smoke including sodium aerosol, and cannot distinguish a sodium fire from a conventional fire; the sodium ionization type detector is mainly applied to smoke detection of sodium-containing aerosol in inert gas, because other components in the air are also ionized when the sampling gas is discharged, the detection accuracy is influenced; the differential pressure detector measures the differential pressure of the sampled gas before and after passing through the filter device, and the method has slow response, delay and larger flow of the sampled gas; the methods are not specially used for detecting sodium aerosol, and early sodium leakage detection cannot be realized. The flame furnace atomization detector generally adopts organic gas combustion flame to carry out atomization treatment on sampled gas, and measures the concentration of sodium element in the gas by measuring the characteristic spectral line intensity of the sodium element, so that early detection of sodium leakage can be realized, but extra fire hazard sources are added by introducing the organic gas into a reactor, the potential safety hazard is larger, the method is adopted by an early French Fenghuang reactor as a main method and a detection means for early detection of LBB sodium leakage, but the requirement on nuclear safety is increasingly enhanced, and the method is gradually faded out for use due to the introduction of the organic gas and the increase of other fire risks, so far, no better method and measurement means are used for replacing the method; the laser detector adopts high-energy laser pulses to dissociate the sampled gas to form a high-temperature plasma state, and obtains sodium element concentration information by detecting and analyzing the intensity of a sodium characteristic spectral line in the plasma cooling process, so that early sodium leakage detection can be realized.
SUMMERY OF THE UTILITY MODEL
Objects of the invention
In order to overcome the defects of the prior art, the on-line detection device for the sodium aerosol in the air has the advantages of long-term stable operation, low energy consumption and low detection limit.
(II) technical scheme
An on-line detection device for sodium aerosol in air, comprising: the device comprises a sampling and shunting device, an atomic emission spectrum excitation source, a spectrum monitoring device and a correction bottle;
wherein the sampling shunt device delivers the air sample to the atomic emission spectroscopy excitation source; the atomic emission spectrum excitation source excites sodium aerosol in an air sample to form an atomic emission spectrum, and the atomic emission spectrum is collected through a spectrum monitoring device; the spectrum monitoring device separates the emitted light of the sodium atoms and converts the light into an electric signal; the calibration vial provides an aerosol sample of known concentration to an atomic emission spectroscopy excitation source.
The sampling and shunting device comprises; a sampling pump and a shunt device;
the sampling pump is connected with a shunt device, and the shunt device is connected with an atomic emission spectrum excitation source.
The atomic emission excitation source includes: the device comprises a power source, an energy conversion device, a working gas flow control component and a working gas source;
wherein the power source is connected with an energy conversion device; and the working gas source is connected to the energy conversion device through the working gas flow control component.
The spectrum monitoring device comprises: a spectrum collection part, a light splitting part and a detector;
the spectrum collecting component is connected with the light splitting component through an optical fiber; the light splitting component is connected with the detector.
The atomic emission excitation source further includes: an ignition device and adopts automatic control ignition.
A plasma cavity is also arranged above the energy conversion device.
The power source is a microwave power source.
The energy conversion device is a microwave plasma rectangular tube.
The spectrum collection component is a reflective collimator.
The detector is a mini fiber spectrometer with a Cheney-Telner structure matched with a linear CCD detector for light splitting and spectrum detection.
The microwave plasma rectangular tube is a triple concentric tube structure of a stainless steel inner tube, a copper middle tube and a copper outer tube.
The outer diameter of the stainless steel inner tube is 2-3 mm, and the wall thickness is 0.3-0.4 mm; the outer diameter of the copper medium pipe is 7-9 mm, and the wall thickness is 0.8-1.0 mm; the outer diameter of the copper outer pipe is 25-27 mm, and the wall thickness is 1.5-2.0 mm.
(III) advantageous effects
The online detection device for sodium aerosol in air adopts atomic emission spectroscopy as a basic principle, and realizes the characteristic of uninterrupted online detection by sampling the sodium aerosol continuously by a sampling pump; meanwhile, the atomic emission spectrum excitation source of the detection device disclosed by the disclosure adopts a microwave plasma device, so that the detection device disclosed by the disclosure has the advantages of low energy consumption and long-term stable operation.
The on-line detection device for sodium aerosol in air is provided with the correction bottle, and a sodium aerosol concentration-spectral intensity standard curve with known concentration is prepared and is a basis for quantitative analysis, so that whether the sodium aerosol in air exists or not and a specific concentration value are detected on line.
Drawings
FIG. 1 is a schematic view of an on-line detection device for sodium aerosol in air;
FIG. 2 is a sodium atomic emission spectrum of sodium aerosol with different concentrations;
wherein A is a sampling shunt device; b atomic emission spectrum excitation source; c, a spectrum monitoring device; 1, a sampling pump; 2, a flow dividing device; 3 working gas source; 4 a working gas flow rate control means; 5 a power source; 6 an energy conversion device; 7 a plasma chamber; 8 a spectrum collection part; 9 a light splitting part; 10, a detector; 11, a correction bottle;
Detailed Description
For better illustration of the technical solution of the present disclosure, the following detailed description is provided with reference to the accompanying drawings:
the disclosed online detection device for sodium aerosol in air takes microwave plasma atomic emission spectroscopy as a technical principle, adopts a pump 1 to uninterruptedly sample environmental gas of a region to be detected, then shunts the aerosol to enter an emission spectrum excitation source, obtains the sodium atomic emission spectroscopy through the excitation process of gasification and atomization, collects emitted light by a reflection-type spectrum collecting mirror and couples the emitted light to an optical fiber, realizes light splitting and detection by a small-sized optical fiber spectrometer, judges whether the sodium aerosol exists in the environmental air of the region to be detected in real time according to spectral information, and further analyzes the content of the sodium aerosol. The method has the characteristic of continuous online monitoring.
Example 1
The sampling and flow-dividing device 2 in the embodiment samples the air of the sample in the area to be measured by using the pump 1, the sampling flow rate is 10L/min, the collected large-flow sample is divided and then flows into the working gas, and then the large-flow sample enters the plasma torch tube simultaneously and is excited by plasma flame to generate the atomic emission spectrum.
And an atomic emission spectrum excitation source B. In order to realize real-time online detection, a plasma device capable of working stably for a long time is generally used, and in this embodiment, a stable and reliable low-power-consumption microwave plasma is used as an excitation source. The working principle of microwave plasma can be described simply as follows: the microwave power source generates microwave power, the microwave power is fed into the microwave torch tube through the coaxial cable, the argon gas source of the working gas absorbs microwave energy, the ignition device generates seed electrons at the moment, plasma is generated rapidly, and the working gas brings a sample into a plasma area to be excited to generate a spectrum.
The atomic emission spectrum excitation source B comprises a microwave power source, an ignition device, a plasma torch tube, a plasma chamber 7, a microwave transmission cable and the like. The microwave plasma torch has the function of inputting energy to the plasma torch tube through the microwave power source to form working gas plasma for exciting a sample to be tested. The microwave power source is an energy supply system of a microwave system, and a small microwave source is selected in the embodiment. The microwave plasma torch tube is a device for realizing energy conversion, and in the embodiment, the microwave plasma torch tube adopting a triple concentric tube structure is composed of a stainless steel inner tube, a copper middle tube and a copper outer tube, wherein the stainless steel inner tube has an outer diameter of 2.7mm and a wall thickness of 0.35mm, the copper middle tube has an outer diameter of 7.5mm and a wall thickness of 0.85mm, and the copper outer tube has an outer diameter of 25mm and a wall thickness of 1.6mm, so that stable microwave plasma can be generated and maintained for sample excitation when microwave power is input. The microwave transmission cable is used for transmitting microwaves, and the device adopts a coaxial cable with the impedance of 50 omega and a special N-type connector with the impedance of 50 omega as transmission media. The plasma chamber 7 has the function of shielding microwave radiation and is arranged above the plasma torch tube. The embodiment utilizes the small-sized high-voltage discharge module to carry out transient pulse discharge to generate seed electrons, so that the plasma is rapidly generated, and automatic control ignition can be realized through instrument software control.
In the instrument of the present embodiment, the reflective collimator is used as an optical collecting device, the generated atomic emission spectrum is collected and coupled into an optical fiber, and a mini optical fiber spectrometer with a cheney-te nano structure is used in combination with a linear CCD detector to perform light splitting and spectrum detection. The spectrum detection at the resolution of 0.2nm can be realized in the range of 560-610 nm.
The calibration vial 11 in this embodiment is a device capable of providing a sample of sodium aerosol of known concentration.
The embodiment utilizes the industrial computer and the control system based on stm32 to realize setting working parameters through instrument software, thereby automatically monitoring the level of sodium aerosol, and viewing the monitoring result in real time through a display screen interface. After the online detection device for the sodium aerosol in the air is adjusted, the detection is carried out according to the following steps:
1. before analyzing a sample, the atomic emission spectroscopy excitation source B needs to be maintained to stably work, in this embodiment, the instrument working gas source 3 is argon, the excitation source is a microwave plasma torch, and high-temperature, high-energy and stable argon plasma can be generated in a normal working state, so that the instrument has a direct excitation capability for sodium aerosol particles. The microwave working power is between 150W, and the flow rate of the working gas is between 800 mL/min.
2. The sampling and shunting device A samples the air of a sample in a region to be detected by utilizing a diaphragm pump integrated in an instrument, the sampling flow rate is 10L/min, then shunts the collected large-flow sample, converges the sample into working gas, and simultaneously enters a plasma torch tube to be excited by plasma flame to generate atomic emission spectrum.
3. In the embodiment, two sodium atom emission characteristic spectral lines at 588.995nm and 589.592nm are taken as bases to judge whether the collected sample contains sodium aerosol.
4. The calibration bottle 11 provides sodium aerosols of different concentrations and known concentrations. And analyzing the sodium aerosol with different concentrations, and establishing a concentration-spectral intensity standard curve as a quantitative analysis basis.
5. And calculating the concentration of the sodium aerosol according to the established concentration-spectral intensity standard curve and the measured emission line intensity of the sodium element.
By the above method, the content of Na with the concentration of 10ppb and 25ppb+/H2The detection result of the O standard sample is shown in FIG. 2.
Example 2
The difference between the present embodiment and embodiment 1 is that the stainless steel inner tube of the triple concentric tube structure microwave plasma torch tube adopted in the present embodiment has an outer diameter of 2mm and a wall thickness of 0.3mm, the copper middle tube has an outer diameter of 7mm and a wall thickness of 0.8mm, and the copper outer tube has an outer diameter of 27mm and a wall thickness of 2 mm;
the microwave working power is between 100W, and the flow rate of the working gas is between 600 mL/min.
By the above method, the concentration of Na is 50ppb and 75ppb+/H2The detection result of the O standard sample is shown in FIG. 2.
Example 3
The difference between the present embodiment and embodiment 1 is that the stainless steel inner tube of the triple concentric tube structure microwave plasma torch tube adopted in the present embodiment has an outer diameter of 3mm and a wall thickness of 0.4mm, the copper middle tube has an outer diameter of 8mm and a wall thickness of 1.0mm, and the copper outer tube has an outer diameter of 26mm and a wall thickness of 1.5 mm;
the microwave working power is between 200W, and the flow rate of the working gas is between 1000 mL/min.
For Na having a concentration of 100ppb by the above-mentioned method+/H2The detection result of the O standard sample is shown in FIG. 2.
It will be apparent to those skilled in the art that various changes and modifications can be made in the present disclosure without departing from the spirit and scope of the disclosure. Thus, if such modifications and variations to the present disclosure fall within the scope of the claims of the present disclosure and their equivalents, it is intended that the present disclosure also encompass such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present disclosure, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the disclosure should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims are intended to be included within the scope of the disclosure.

Claims (12)

1. An on-line detection device for sodium aerosol in air, which is characterized by comprising: the device comprises a sampling and shunting device (A), an atomic emission spectrum excitation source (B), a spectrum monitoring device (C) and a correction bottle (11);
wherein the sampling diverter (A) delivers an air sample to an atomic emission spectroscopy excitation source (B); the atomic emission spectrum excitation source (B) excites sodium aerosol in an air sample to form an atomic emission spectrum, and the atomic emission spectrum is collected through the spectrum monitoring device (C); the spectrum monitoring device (C) separates the emitted light of the sodium atoms and converts the light into an electric signal; the calibration bottle (11) provides aerosol samples with known concentrations for the atomic emission spectroscopy excitation source (B).
2. The on-line detection device for sodium aerosol in air according to claim 1, wherein the sampling shunt device comprises; a sampling pump (1) and a shunt device (2);
the sampling pump (1) is connected with a shunt device (2), and the shunt device (2) is connected with an atomic emission spectrum excitation source (B).
3. The on-line detection device of claim 1, wherein the atomic emission excitation source comprises: the device comprises a power source (5), an energy conversion device (6), a working gas flow control component (4) and a working gas source (3);
wherein the power source (5) is connected with an energy conversion device (6); and the working gas source (3) is connected to the energy conversion device (6) through a working gas flow control component (4).
4. An on-line detection device for sodium aerosol in air according to claim 1, characterized in that the spectrum monitoring device (C) comprises: a spectrum collection component (8), a light splitting component (9) and a detector (10);
wherein the spectrum collecting part (8) is connected with the light splitting part (9) through an optical fiber; the light splitting component (9) is connected with a detector (10).
5. The on-line detection device of claim 3, wherein the atomic emission excitation source further comprises: an ignition device and adopts automatic control ignition.
6. The on-line detection device for sodium aerosol in air according to claim 3, characterized in that a plasma chamber (7) is further arranged above the energy conversion device (6).
7. An on-line detection device for sodium aerosol in air according to claim 3, characterized in that the power source (5) is a microwave power source.
8. The on-line detection device for sodium aerosol in air according to claim 3, wherein the energy conversion device (6) is a microwave plasma rectangular tube.
9. An on-line detection device for sodium aerosol in air according to claim 4, characterized in that the spectrum collecting component (8) is a reflective collimator.
10. The on-line detection device for sodium aerosol in air according to claim 4, wherein the detector (10) is a Cheney-Telner structure micro fiber spectrometer matched with a linear CCD detector for light splitting and spectrum detection.
11. The on-line detection device for sodium aerosol in air according to claim 8, wherein the microwave plasma rectangular tube is a triple concentric tube structure of a stainless steel inner tube, a copper middle tube and a copper outer tube.
12. The on-line detection device for sodium aerosol in air according to claim 11, wherein the outer diameter of the stainless steel inner tube is 2-3 mm, and the wall thickness is 0.3-0.4 mm; the outer diameter of the copper medium pipe is 7-9 mm, and the wall thickness is 0.8-1.0 mm; the outer diameter of the copper outer pipe is 25-27 mm, and the wall thickness is 1.5-2.0 mm.
CN201921087733.8U 2019-07-12 2019-07-12 On-line detection device for sodium aerosol in air Active CN211318204U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110320203A (en) * 2019-07-12 2019-10-11 中国原子能科学研究院 Sodium aerosol on-line water flushing device and method in a kind of air
CN117074332A (en) * 2022-05-10 2023-11-17 天津师范大学 Method for monitoring bioaerosol particles

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110320203A (en) * 2019-07-12 2019-10-11 中国原子能科学研究院 Sodium aerosol on-line water flushing device and method in a kind of air
CN117074332A (en) * 2022-05-10 2023-11-17 天津师范大学 Method for monitoring bioaerosol particles
CN117074332B (en) * 2022-05-10 2024-06-11 天津师范大学 Method for monitoring bioaerosol particles

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