CN107727642B - Laser detection method for heavy metal elements in atmospheric particulates - Google Patents
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Abstract
The invention belongs to the technical field of atmospheric pollution detection, and particularly relates to a laser detection method for heavy metal elements in atmospheric particulates, which comprises the following steps: step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected; step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination; step 3, pressing the filter plate to obtain a sample plate; step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma; and 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and the content of the heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere. The invention adopts the solid inorganic filter plate, and can solve the problems of limited signal intensity and difficult accurate collection and analysis in the current atmospheric laser detection process.
Description
Technical Field
The invention belongs to the technical field of atmospheric pollution detection, and particularly relates to a laser detection method for heavy metal elements in atmospheric particulates.
Background
At present, with the rapid development of industry and economy and the rapid increase of population, heavy metal pollution in the atmosphere becomes one of the main pollution faced by the world at present, and the heavy metal pollution mainly comes from harmful gas and dust containing a large amount of heavy metals generated by industrial production, motor vehicle tail gas, mining, boiler coal burning and automobile tire abrasion. Heavy metal pollutants are mainly attached to PM2.5 and PM10 particles, and PM2.5 and PM10 refer to inhalable particles with aerodynamic equivalent diameters of less than or equal to 2.5 microns and 10 microns, the inhalable particles have strong adsorption capacity, are carriers and catalysts of various pollutants including heavy metal elements, and can stay in the atmosphere for a long time and be transmitted remotely. Heavy metal pollutants are difficult to degrade in natural atmospheric environment, can be accumulated in animals and plants for a long time, are gradually enriched through food chains, can be increased by tens of hundreds or even tens of thousands of times in concentration, finally enter a human body and are deposited in the lung to directly participate in blood circulation, and have great harm degree to the human body.
At present, the common method for detecting heavy metal elements in atmospheric aerosol is as follows: the atmosphere is sampled on site and then sent to a relevant laboratory for measurement by Atomic Absorption Spectroscopy (AAS), inductively coupled plasma spectroscopy (ICP-AES), Atomic Fluorescence Spectroscopy (AFS), or the like. These analysis methods all require a series of processes such as sample collection, preparation, assay, etc., and usually the detection results can be obtained after several hours or even days, and the method of sampling at intervals can only reflect the heavy metal content in the atmosphere within a short period of time, so that the detection results deviate from the actual sample conditions to generate certain errors.
The laser induced breakdown spectroscopy (L IBS) technology has the characteristics of no need of preprocessing the sample, realization of simultaneous detection of multiple elements and effective solution of the difficult problem of online, real-time and continuous monitoring of multiple heavy metal elements in atmospheric suspended pollution particles.
The atmosphere is used as a sample existing in a gaseous form, if the atmosphere is directly sampled, a pulse laser beam acts on the atmosphere sample, the intensity of the plasma spectrum signal generated by laser-induced breakdown is very limited, the spectrum signal acquisition device is difficult to effectively collect and analyze, the intensity of the spectrum signal fluctuates violently, even if the gas with fixed content is measured under a stable condition, the signal can present a wider intensity distribution, and the weakness enables the laser-induced breakdown spectroscopy (L IBS) technology to be limited in the aspect of quantitative detection of the gas sample.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a laser detection method for heavy metal elements in atmospheric particulates, which adopts a solid inorganic filter plate to solve the problems that the signal intensity is limited and accurate collection and analysis are difficult in the existing atmospheric laser detection process.
In order to achieve the technical purpose, the technical scheme of the invention is as follows: a laser detection method for heavy metal elements in atmospheric particulates comprises the following steps:
step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected;
step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination;
step 3, pressing the filter plate to obtain a sample plate;
step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma;
and 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and the content of the heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere.
Preferably, the filter plate in the step 2 is a siliceous inorganic filter material, and has pores of 1 micron, a diameter of 30mm and a thickness of 3 mm.
Preferably, the laser parameters in step 4 are as follows: light source: nd: YAG laser, single pulse energy is 50mJ, and pulse width is 6 ns.
Preferably, the formulation of the siliceous inorganic filter material is as follows:
10-24 parts of silicon dioxide, 2-4 parts of foaming agent, 1-3 parts of penetrating agent, 35-45 parts of solvent, 10-15 parts of adhesive and 2-4 parts of dispersing agent.
As an improvement, the foaming agent adopts sodium dodecyl sulfate.
As an improvement, the dispersing agent adopts polyvinylpyrrolidone or polyethylene glycol.
As an improvement, the solvent adopts ethanol or ethanol water solution with the ethanol concentration of 50-80%.
As a modification, the adhesive adopts epoxy modified silicone resin or methyl silicone resin.
As an improvement, the penetrant adopts fatty alcohol-polyoxyethylene ether or alkylphenol polyoxyethylene ether.
As an improvement, the preparation method of the siliceous inorganic filter material comprises the following steps:
step 1, adding silicon dioxide into a solvent, then adding a dispersing agent, and ultrasonically stirring until the silicon dioxide is completely dissolved;
step 2, mixing the adhesive with the foaming agent and the penetrating agent, and mechanically stirring to obtain a mixed solution;
step 3, adding the mixed solution into the stirring solution obtained in the step 1, and continuing to perform ultrasonic stirring until the mixed solution is completely dispersed;
step 4, carrying out reduced pressure distillation reaction on the dispersed solution for 2-4h, and then carrying out pressure molding reaction for 2-4h to obtain a rough blank;
and 5, sintering the rough blank in a muffle furnace for 4-8 hours to obtain the siliceous filtering material.
As a further improvement, the ultrasonic frequency in the step 1 is 1.4-5.5kHz, the mechanical stirring speed in the step 2 is 2000-4000r/min, the ultrasonic stirring in the step 3 adopts constant-temperature stirring, the pressure of reduced pressure distillation in the step 4 is 50-80% of the atmospheric pressure, the temperature is 80-110 ℃, the pressure of a pressure die is 10-20MPa, the pressure is 90-110 ℃, the sintering temperature in the step 5 is 300-400 ℃, and the sintering temperature rise mode is as follows:
from the above description, it can be seen that the present invention has the following advantages:
1. the invention adopts the solid inorganic filter plate, and can solve the problems of limited signal intensity and difficult accurate collection and analysis in the current atmospheric laser detection process.
2. The invention adopts the siliceous inorganic filter plate, can effectively and accurately collect the particles in the gas, has stable and single structure, high accuracy of the measurement result and good repeatability.
3. The invention adopts the micron-sized siliceous inorganic filter plate which can adsorb most of PM2.5 and PM10 suspended particles.
4. The invention provides a formula and a preparation method of a siliceous inorganic filter plate, wherein materials are completely mixed in a reduced pressure distillation mode, a compression molding mode is adopted for pressing to form a dense structure with a size, a dense structure can be formed in a gradient sintering mode, and the formation of micron-sized pores is ensured.
Detailed Description
The following is a specific embodiment of the present invention, but is not intended to limit the claims of the present invention in any way.
Example 1
A laser detection method for heavy metal elements in atmospheric particulates is characterized by comprising the following steps: the method comprises the following steps:
step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected;
step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination;
step 3, pressing the filter plate to obtain a sample plate;
step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma;
and 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and the content of the heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere.
The filter plate in the step 2 adopts a siliceous inorganic filter material, the pores are 1 micron, the diameter is 30mm, and the thickness is 3 mm.
The laser parameters in the step 4 are as follows: light source: nd: YAG laser, single pulse energy is 50mJ, and pulse width is 6 ns.
The formula of the siliceous inorganic filter material is as follows:
10 parts of silicon dioxide, 2 parts of foaming agent, 1 part of penetrating agent, 35 parts of solvent, 10 parts of adhesive and 2 parts of dispersing agent.
The foaming agent adopts sodium dodecyl sulfate.
The dispersing agent adopts polyvinylpyrrolidone.
The solvent is ethanol.
The adhesive is epoxy modified organic silicon resin.
The penetrating agent is fatty alcohol-polyoxyethylene ether.
The preparation method of the siliceous inorganic filter material comprises the following steps:
step 1, adding silicon dioxide into a solvent, then adding a dispersing agent, and ultrasonically stirring until the silicon dioxide is completely dissolved;
step 2, mixing the adhesive with the foaming agent and the penetrating agent, and mechanically stirring to obtain a mixed solution;
step 3, adding the mixed solution into the stirring solution obtained in the step 1, and continuing to perform ultrasonic stirring until the mixed solution is completely dispersed;
step 4, carrying out reduced pressure distillation reaction on the dispersed solution for 2 hours, and then carrying out pressure molding reaction for 2-4 hours to obtain a rough blank;
and 5, sintering the rough blank in a muffle furnace for 4 hours to obtain the siliceous filtering material.
The ultrasonic frequency in the step 1 is 1.4kHz, the mechanical stirring speed in the step 2 is 2000r/min, the ultrasonic stirring in the step 3 adopts constant-temperature stirring, the pressure of reduced pressure distillation in the step 4 is 50% of the atmospheric pressure, the temperature is 80 ℃, the pressure of a pressure die is 10MPa, the pressure is 90 ℃, the sintering temperature in the step 5 is 300 ℃, and the sintering temperature rising mode is as follows:
| temperature of | Time of day |
| At room temperature | 20min |
| 150℃ | 60min |
| 250℃ | 10min |
| 300℃ | 2.5h |
Example 2
A laser detection method for heavy metal elements in atmospheric particulates is characterized by comprising the following steps: the method comprises the following steps:
step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected;
step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination;
step 3, pressing the filter plate to obtain a sample plate;
step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma;
and 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and the content of the heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere.
The filter plate in the step 2 adopts a siliceous inorganic filter material, the pores are 1 micron, the diameter is 30mm, and the thickness is 3 mm.
The laser parameters in the step 4 are as follows: light source: nd: YAG laser, single pulse energy is 50mJ, and pulse width is 6 ns.
The formula of the siliceous inorganic filter material is as follows:
24 parts of silicon dioxide, 4 parts of foaming agent, 3 parts of penetrating agent, 45 parts of solvent, 15 parts of adhesive and 4 parts of dispersing agent.
The foaming agent adopts sodium dodecyl sulfate.
The dispersing agent adopts polyethylene glycol.
The solvent adopts ethanol water solution with the ethanol concentration of 50 percent.
The adhesive is methyl silicone resin.
The penetrating agent adopts alkylphenol polyoxyethylene.
The preparation method of the siliceous inorganic filter material comprises the following steps:
step 1, adding silicon dioxide into a solvent, then adding a dispersing agent, and ultrasonically stirring until the silicon dioxide is completely dissolved;
step 2, mixing the adhesive with the foaming agent and the penetrating agent, and mechanically stirring to obtain a mixed solution;
step 3, adding the mixed solution into the stirring solution obtained in the step 1, and continuing to perform ultrasonic stirring until the mixed solution is completely dispersed;
step 4, carrying out reduced pressure distillation reaction on the dispersed solution for 4h, and then carrying out pressure molding reaction for 4h to obtain a rough blank;
and 5, sintering the rough blank in a muffle furnace for 8 hours to obtain the siliceous filtering material.
The ultrasonic frequency in the step 1 is 5.5kHz, the mechanical stirring speed in the step 2 is 4000r/min, the ultrasonic stirring in the step 3 adopts constant-temperature stirring, the pressure of reduced pressure distillation in the step 4 is 80% of the atmospheric pressure, the temperature is 110 ℃, the pressure of a pressure die is 20MPa, the pressure is 110 ℃, the sintering temperature in the step 5 is 400 ℃, and the sintering temperature rising mode is as follows:
| temperature of | Time of day |
| 150℃ | 30min |
| 250℃ | 120min |
| 400℃ | 5.5h |
Example 3
A laser detection method for heavy metal elements in atmospheric particulates is characterized by comprising the following steps: the method comprises the following steps:
step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected;
step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination;
step 3, pressing the filter plate to obtain a sample plate;
step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma;
and 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and the content of the heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere.
The filter plate in the step 2 adopts a siliceous inorganic filter material, the pores are 1 micron, the diameter is 30mm, and the thickness is 3 mm.
The laser parameters in the step 4 are as follows: light source: nd: YAG laser, single pulse energy is 50mJ, and pulse width is 6 ns.
The formula of the siliceous inorganic filter material is as follows:
20 parts of silicon dioxide, 3 parts of foaming agent, 2 parts of penetrating agent, 40 parts of solvent, 12 parts of adhesive and 3 parts of dispersing agent.
The foaming agent adopts sodium dodecyl sulfate.
The dispersing agent adopts polyvinylpyrrolidone.
The solvent adopts an ethanol water solution with the ethanol concentration of 80 percent.
The adhesive is epoxy modified organic silicon resin.
The penetrating agent is fatty alcohol-polyoxyethylene ether.
The preparation method of the siliceous inorganic filter material comprises the following steps:
step 1, adding silicon dioxide into a solvent, then adding a dispersing agent, and ultrasonically stirring until the silicon dioxide is completely dissolved;
step 2, mixing the adhesive with the foaming agent and the penetrating agent, and mechanically stirring to obtain a mixed solution;
step 3, adding the mixed solution into the stirring solution obtained in the step 1, and continuing to perform ultrasonic stirring until the mixed solution is completely dispersed;
step 4, carrying out reduced pressure distillation reaction on the dispersed solution for 3h, and then carrying out pressure molding reaction for 3h to obtain a rough blank;
and 5, sintering the rough blank in a muffle furnace for 6 hours to obtain the siliceous filtering material.
The ultrasonic frequency in the step 1 is 3.5kHz, the mechanical stirring speed in the step 2 is 3000r/min, the ultrasonic stirring in the step 3 adopts constant-temperature stirring, the pressure of reduced pressure distillation in the step 4 is 70% of the atmospheric pressure, the temperature is 100 ℃, the pressure of a pressure die is 15MPa, the pressure temperature is 105 ℃, the sintering temperature in the step 5 is 350 ℃, and the sintering temperature rise mode is as follows:
| temperature of | Time of day |
| 80℃ | 30min |
| 200℃ | 60min |
| 250℃ | 30min |
| 350℃ | 4h |
In summary, the invention has the following advantages:
1. the invention adopts the solid inorganic filter plate, and can solve the problems of limited signal intensity and difficult accurate collection and analysis in the current atmospheric laser detection process.
2. The invention adopts the siliceous inorganic filter plate, can effectively and accurately collect the particles in the gas, has stable and single structure, high accuracy of the measurement result and good repeatability.
3. The invention adopts the micron-sized siliceous inorganic filter plate which can adsorb most of PM2.5 and PM10 suspended particles.
4. The invention provides a formula and a preparation method of a siliceous inorganic filter plate, wherein materials are completely mixed in a reduced pressure distillation mode, a compression molding mode is adopted for pressing to form a dense structure with a size, a dense structure can be formed in a gradient sintering mode, and the formation of micron-sized pores is ensured.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (2)
1. A laser detection method for heavy metal elements in atmospheric particulates is characterized by comprising the following steps: the method comprises the following steps:
step 1, collecting gas by using a gas collecting device to obtain sample gas to be detected;
step 2, passing the sample gas to be detected through a filter plate, and attaching gas suspended particles to the filter plate to form a stable filtering lamination;
step 3, pressing the filter plate to obtain a sample plate;
step 4, focusing the pulse laser beam output by the laser on the surface of the sample plate through a focusing lens to form high-temperature plasma;
step 5, analyzing the plasma spectrum signal through a spectrum detection system to obtain the information of the type and content of heavy metal elements in the atmosphere suspended polluted particles so as to determine the heavy metal pollution degree of the atmosphere; the filter plate in the step 2 adopts a siliceous inorganic filter material, the pores are 1 micron, the diameter is 30mm, and the thickness is 3 mm;
the laser parameters in the step 4 are as follows: light source: nd: YAG laser, single pulse energy is 50mJ, pulse width is 6 ns;
the formula of the siliceous inorganic filter material is as follows:
10-24 parts of silicon dioxide, 2-4 parts of foaming agent, 1-3 parts of penetrating agent, 35-45 parts of solvent, 10-15 parts of adhesive and 2-4 parts of dispersing agent;
the foaming agent adopts sodium dodecyl sulfate; the dispersing agent adopts polyvinylpyrrolidone or polyethylene glycol; the solvent is ethanol or ethanol water solution with the ethanol concentration of 50-80%; the adhesive is epoxy modified organic silicon resin or methyl silicon resin; the penetrating agent adopts fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether.
2. The laser detection method of the heavy metal elements in the atmospheric particulates according to claim 1, characterized in that: the preparation method of the siliceous inorganic filter material comprises the following steps:
step 1, adding silicon dioxide into a solvent, then adding a dispersing agent, and ultrasonically stirring until the silicon dioxide is completely dissolved;
step 2, mixing the adhesive with the foaming agent and the penetrating agent, and mechanically stirring to obtain a mixed solution;
step 3, adding the mixed solution into the stirring solution obtained in the step 1, and continuing to perform ultrasonic stirring until the mixed solution is completely dispersed;
step 4, carrying out reduced pressure distillation reaction on the dispersed solution for 2-4h, and then carrying out pressure molding reaction for 2-4h to obtain a rough blank;
and 5, sintering the rough blank in a muffle furnace for 4-8 hours to obtain the siliceous filtering material.
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| CN109085151A (en) * | 2018-09-11 | 2018-12-25 | 南京信息工程大学 | The on-line measuring device and detection method of a kind of atmosphere pollution mercury and its isotope |
| CN109632588B (en) * | 2018-12-30 | 2024-03-12 | 江苏苏净集团有限公司 | Device and method for detecting pollution of oil particulate matters |
Citations (4)
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|---|---|---|---|---|
| EP0826412A3 (en) * | 1996-08-26 | 1999-06-02 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Berlin | Method for producing filter elements and the filter elements thus produced |
| CN103487427A (en) * | 2013-09-27 | 2014-01-01 | 苏州国环环境检测有限公司 | Method for detecting metallic elements in atmospheric exhaust gas particulates |
| CN204330594U (en) * | 2014-12-17 | 2015-05-13 | 郭锐 | A kind of atmosphere heavy metal pollution thing collecting and detecting device based on LIBS |
| CN205691507U (en) * | 2016-04-14 | 2016-11-16 | 浙江师范大学 | The highly sensitive quantitative testing device of heavy metal element in a kind of atmospheric aerosol |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0826412A3 (en) * | 1996-08-26 | 1999-06-02 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Berlin | Method for producing filter elements and the filter elements thus produced |
| CN103487427A (en) * | 2013-09-27 | 2014-01-01 | 苏州国环环境检测有限公司 | Method for detecting metallic elements in atmospheric exhaust gas particulates |
| CN204330594U (en) * | 2014-12-17 | 2015-05-13 | 郭锐 | A kind of atmosphere heavy metal pollution thing collecting and detecting device based on LIBS |
| CN205691507U (en) * | 2016-04-14 | 2016-11-16 | 浙江师范大学 | The highly sensitive quantitative testing device of heavy metal element in a kind of atmospheric aerosol |
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