CN110411907B - Method, system and medium for measuring coagulation efficiency of submicron particles on plant leaves - Google Patents
Method, system and medium for measuring coagulation efficiency of submicron particles on plant leaves Download PDFInfo
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- CN110411907B CN110411907B CN201910533658.1A CN201910533658A CN110411907B CN 110411907 B CN110411907 B CN 110411907B CN 201910533658 A CN201910533658 A CN 201910533658A CN 110411907 B CN110411907 B CN 110411907B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N2015/0277—Average size only
Abstract
The invention provides a method, a system and a medium for measuring the coagulation efficiency of submicron particles on plant leaves, which comprises the following steps: preparing particles: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0(ii) a Simulating a dust retention step: the method comprises the following steps of pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time. Compared with the traditional method for measuring the particle size of the leaf surface particles, the method has the advantages that the defects of small visual field range, incapability of separating water-soluble components and the like can be overcome by using the X-ray microscope, the three-dimensional imaging with high precision and larger visual field can be realized, the data of each particle in all the structures of the leaf can be accurately obtained by combining software, the observation is more visual, and the particle size calculation is more scientific and reliable.
Description
Technical Field
The invention relates to the field of plant surface physical properties, in particular to a method, a system and a medium for measuring the coagulation efficiency of submicron particles on plant leaves. In particular to a method for measuring the particle size of submicron particles on plant leaves by using an X-ray microscope so as to calculate the coagulation efficiency of the particles on the leaf surfaces.
Background
In recent years, with the rapid development of urbanization, the problem of air pollution becomes more and more prominent, and aerosol particles in the atmosphere become the primary pollutants for pollution prevention and control. The particles with the particle size range of 0.1-1 μm are also called submicron particles, and are not easy to diffuse like ultrafine particles with smaller particle sizes, and have higher gravity settling velocity like micron-sized particles with larger particle sizes, so that the dust removal method is a difficult point for dust removal, and therefore, the method has important significance for preventing and controlling haze weather by paying attention to the transmission and purification processes of the submicron particles in the air.
The reduction of atmospheric particulates by plants is an important means for preventing and controlling atmospheric pollution, and the process is generally considered to be realized by dry sedimentation, namely a process that the atmospheric particulates collide with the plants or are retained on a contact surface after contacting the plants so as to be separated from the atmospheric environment. In the field of plant dust retention, people mostly pay attention to the research on the dry settling rate of different plants under different conditions, namely the dust retention amount of the plants. But neglects to explain the transformation law and action mechanism of the migration of particulate matter on the air-plant interface.
The plant dust retention process is not a simple process that particles fall on the surface of a leaf in an original form, the particles collide or adhere to each other under the action of external force to be agglomerated into larger particles, namely, the agglomeration effect occurs, the agglomeration effect can be described by the agglomeration efficiency α, namely, the average particle size ratio of the particles before and after the process, however, the particle size measurement of the particles on the leaf surface is difficult, and the current common methods mainly comprise a scanning electron microscope method and a washing-different-aperture filter membrane filtration method.
Patent document CN104722340B (application number: 201510093611.X) discloses an artificial aerosol climate box and a use method thereof, the artificial aerosol climate box comprises a stainless steel shell and the like, a closed tank body is positioned in the stainless steel shell, a variable speed fan, a material box and an annular air flushing pipeline are sequentially positioned in the closed tank body from bottom to top, a double-opening type sample feeding box is positioned in the material box, an air inlet, a tank body top cover and an operation panel are all fixed on the top end of the stainless steel shell, a reserved detection port is positioned on the tank body top cover, the tank body top cover and the stainless steel shell are fixed through a sealing fixing bolt, and a vacuum pump is positioned in the stainless steel shell and positioned on the side face of the closed tank body.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method, a system and a medium for measuring the coagulation efficiency of submicron particles on plant leaves.
The invention provides a method for measuring the coagulation efficiency of submicron particles on plant leaves, which comprises the following steps:
preparing particles: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
Simulating a dust retention step: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
and (3) coagulation efficiency obtaining step: taking out the dust-retention and adsorbed sample, cutting a small blade block with a preset size, wrapping the small blade block with a sealing film, fixing the bottom of the blade on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and performing quantitative analysis on the three-dimensional image by using image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
Preferably, the particulate preparation step:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0。
Preferably, the simulating dust-holding step:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time, and taking out the blades.
Preferably, the coagulation efficiency obtaining step:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
Preferably, the smoke box comprises: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
the airtight jar of body is located the stainless steel shell, and variable speed fan, annular air wash the pipeline from supreme airtight jar of being located in proper order down internal, and air inlet, jar body top cap, operating panel all fix on the top of stainless steel shell, reserve and detect the mouth and be located a jar body top cap, fix through sealed fixing bolt between jar body top cap and the stainless steel shell, and the vacuum pump is located the stainless steel shell and is located the side of the airtight jar of body.
Preferably, the X-ray microscope comprises any one of:
xradia 520Versa, produced by Zeiss, germany, sub-micron resolution CT which can achieve the same functionality;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
The invention provides a system for measuring the coagulation efficiency of submicron particles on plant leaves, which comprises:
the particle preparation module comprises: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
The simulation dust retention module: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
a coagulation efficiency acquisition module: taking out the dust-retention and adsorbed sample, cutting a small blade block with a preset size, wrapping the small blade block with a sealing film, fixing the bottom of the blade on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and performing quantitative analysis on the three-dimensional image by using image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
Preferably, the particulate preparation module:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0；
The simulation dust retention module:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blade is dried, the hanger is hung in the smoke box bodyHooking, covering the case cover, controlling the environmental conditions in the smog case to meet the requirements, opening the fan to mix the air in the case, flushing the inner wall of the case body by pure nitrogen to enable PM in the case body1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time length, and taking out the blades;
the coagulation efficiency acquisition module:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCThe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
Preferably, the smoke box comprises: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
the sealed tank body is positioned in the stainless steel shell, the variable speed fan and the annular air flushing pipeline are sequentially positioned in the sealed tank body from bottom to top, the air inlet, the tank body top cover and the operation panel are all fixed on the top end of the stainless steel shell, the reserved detection port is positioned on the tank body top cover, the tank body top cover and the stainless steel shell are fixed through a sealing fixing bolt, and the vacuum pump is positioned in the stainless steel shell and positioned on the side face of the sealed tank body;
the X-ray microscope includes any one of:
xradia 520Versa, produced by Zeiss, Germany, can realize the same functional sub-micron resolution CT;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
According to the present invention, there is provided a computer readable storage medium storing a computer program which, when executed by a processor, implements the steps of the method for measuring the coagulation efficiency of submicron particulate matter on plant leaves according to any one of claims 1 to 6.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the traditional method for measuring the particle size of the leaf surface particles, the method has the advantages that the defects of small visual field range, incapability of separating water-soluble components and the like can be overcome by using the X-ray microscope, the three-dimensional imaging with high precision and larger visual field can be realized, the data of each particle in all the structures of the leaf can be accurately obtained by combining software, the observation is more visual, and the particle size calculation is more scientific and reliable.
2. The invention firstly provides the method for measuring the coagulation efficiency of the submicron particles on the plant blade, and the X-ray microscope with high precision, wide visual field and three-dimensional imaging can realize the visual observation and measurement of the particles on the blade, and the processed image can accurately and effectively measure the average particle size of the particles on the blade.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
fig. 1 is a schematic view of the emission particle size distribution of the submicron particulate according to the preferred embodiment of the present invention.
Fig. 2 is a schematic view of scanning camphor tree leaves according to a preferred embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
The invention provides a method for measuring the coagulation efficiency of submicron particles on plant leaves, which comprises the following steps:
preparing particles: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
Simulating a dust retention step: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
and (3) coagulation efficiency obtaining step: taking out the sample after dust retention and adsorption, cutting into small pieces of blades with preset size, wrapping with sealing film, and packaging the bottom of the bladesFixed on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and then carrying out quantitative analysis on the three-dimensional image by utilizing image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
Further, the image processing and three-dimensional reconstruction software is ORS Dragonfly.
Specifically, the particulate preparation step:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0。
Specifically, the dust retention simulation step:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time, and taking out the blades.
Specifically, the coagulation efficiency obtaining step:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
Specifically, the smoke box includes: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
the airtight jar of body is located the stainless steel shell, and variable speed fan, annular air wash the pipeline from supreme airtight jar of being located in proper order down internal, and air inlet, jar body top cap, operating panel all fix on the top of stainless steel shell, reserve and detect the mouth and be located a jar body top cap, fix through sealed fixing bolt between jar body top cap and the stainless steel shell, and the vacuum pump is located the stainless steel shell and is located the side of the airtight jar of body.
Specifically, the X-ray microscope includes any one of:
xradia 520Versa, produced by Zeiss, germany, sub-micron resolution CT which can achieve the same functionality;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
The system for measuring the coagulation efficiency of the submicron particles on the plant leaves can be realized by the steps and the flows of the method for measuring the coagulation efficiency of the submicron particles on the plant leaves. The method for measuring the coagulation efficiency of the submicron particles on the plant leaves can be understood as a preferred example of the system for measuring the coagulation efficiency of the submicron particles on the plant leaves by a person skilled in the art.
The invention provides a system for measuring the coagulation efficiency of submicron particles on plant leaves, which comprises:
the particle preparation module comprises: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
The simulation dust retention module: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
a coagulation efficiency acquisition module: taking out the dust-retention and adsorbed sample, cutting a small blade block with a preset size, wrapping the small blade block with a sealing film, fixing the bottom of the blade on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and performing quantitative analysis on the three-dimensional image by using image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
Specifically, the particulate preparation module:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0；
The simulation dust retention module:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time length, and taking out the blades;
the coagulation efficiency acquisition module:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
Specifically, the smoke box includes: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
further, the smoke box is an artificial aerosol climate box disclosed in patent document CN 104722340B;
the sealed tank body is positioned in the stainless steel shell, the variable speed fan and the annular air flushing pipeline are sequentially positioned in the sealed tank body from bottom to top, the air inlet, the tank body top cover and the operation panel are all fixed on the top end of the stainless steel shell, the reserved detection port is positioned on the tank body top cover, the tank body top cover and the stainless steel shell are fixed through a sealing fixing bolt, and the vacuum pump is positioned in the stainless steel shell and positioned on the side face of the sealed tank body;
the X-ray microscope includes any one of:
xradia 520Versa, produced by Zeiss, Germany, can realize the same functional sub-micron resolution CT;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
According to the present invention, there is provided a computer readable storage medium storing a computer program which, when executed by a processor, implements the steps of the method for measuring the coagulation efficiency of submicron particulate matter on plant leaves according to any one of claims 1 to 6.
The present invention will be described more specifically below with reference to preferred examples.
Preferred example 1:
a method for measuring the coagulation efficiency of submicron particles on plant leaves by using an X-ray microscope is characterized by comprising the following steps of:
s1: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
S2: putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particle concentration condition to enable the sample to carry out dust retention and adsorption for 30 minutes;
s3: after the sample is taken out, a small blade block (about 2mm in width and about 4mm in length) is cut, and the bottom of the blade is fixed on a special sample clamp of an X-ray microscope after being wrapped by a sealing film. Setting relevant parameters of an X-ray microscope, scanning and imaging, and carrying out quantitative analysis on the three-dimensional image by using ORSDragonfly image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
The simulation particulate matter described in the step S1 is a saturated solution of salt, and is required to satisfy the condition that the proportion of particulate matter with the particle size of 0.1-1 μm is more than 95% during emission, and the emission average particle size is D0。
Step S2 specifically includes the following operations: 1) pickingThe fresh plant leaves meeting the experimental requirements are immediately washed away with flowing water repeatedly to remove atmospheric particulates on the surface, and finally washed with pure water once, and then placed in a ventilation environment of clean air to be naturally dried; 2) after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to 5 mu g/m3The following; 3) blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level; 4) after 30 minutes, the dust retention was stopped and the leaves were removed.
Step S3 specifically includes the following operations: 1) carefully cut small pieces of the leaf (about 2mm wide and 4mm long) at specific locations with a knife under a dissecting scope; 2) slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process; 3) fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue; 4) setting relevant parameters of an X-ray microscope, namely voltage of 40-50 kV, power of 3-4W and objective lens multiplying power of 4-40X, and performing three-dimensional scanning imaging; 5) leading the picture into Dragonfly software, screening out the particles contained in the sample, and leading out the volume V of the particlesi4) coagulation efficiency α, i.e., the average particle size ratio before and after coagulation, can be calculated from equation 1:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
The smoke box includes: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump.
The airtight jar of body is located the stainless steel shell, and variable speed fan, annular air wash the pipeline from supreme airtight jar of being located in proper order down internal, and air inlet, jar body top cap, operating panel all fix on the top of stainless steel shell, reserve and detect the mouth and be located a jar body top cap, fix through sealed fixing bolt between jar body top cap and the stainless steel shell, and the vacuum pump is located the stainless steel shell and is located the side of the airtight jar of body.
The X-ray microscope is Xradia 520Versa produced by German Zeiss, can realize lossless three-dimensional structure imaging, has the highest spatial resolution less than or equal to 0.7 mu m and the adjustable voltage range of 30-160 kV, or can be replaced by a CT with submicron resolution which can realize the same function.
Preferred example 2:
aiming at filling the research blank of the coagulation effect of the blade particles and overcoming the defects of the existing particle size determination method, the invention firstly provides a method for directly determining the particle size of submicron particles on the blade by using an X-ray microscope.
The invention is realized by the following technical scheme:
the invention provides a method for measuring coagulation efficiency of submicron particles on plant leaves by using an X-ray microscope, which comprises the following steps:
s1: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
S2: putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particle concentration condition to enable the sample to carry out dust retention and adsorption for 30 minutes;
s3: after the sample is taken out, a small blade block (about 2mm in width and about 4mm in length) is cut, and the bottom of the blade is fixed on a special sample clamp of an X-ray microscope after being wrapped by a sealing film. Setting relevant parameters of an X-ray microscope, scanning and imaging, and carrying out quantitative analysis on the three-dimensional image by using ORSDragonfly image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
Preferably, the simulated particulate matter in step S1 is a saturated solution of salt, and is required to satisfy the condition that the percentage of particulate matter with a particle size of 0.1 to 1 μm is 95% or more during emission.
Preferably, the average particle size of the simulated particles is D when the simulated particles are emitted0。
Preferably, step S2 specifically includes the following operations: 1) picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air; 2) after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to 5 mu g/m3The following; 3) blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level; 4) after 30 minutes, the dust retention was stopped and the leaves were removed.
As a preferable scheme, the step S3 specifically comprises the following operations of 1) carefully cutting a small blade block (with the width of about 2mm and the length of about 4mm) at a specific position by a blade under a dissecting mirror, 2) lightly wrapping the cut small blade block by a sealing film, compacting and fixing the edge of the sealing film along the edge of the blade by a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process, 3) fixing the bottom of the blade on a special sample clamp of an X-ray microscope by special glue, 4) setting relevant parameters of the X-ray microscope, namely the voltage of 40-50 kV, the power of 3-4W and the magnification of an objective lens of 4-40X, carrying out three-dimensional scanning imaging, 5) introducing ORSDragon fly image processing and three-dimensional reconstruction software to screen out the particulate matters contained in the sample and lead out the volume Vi of the particulate matters, and 4) coagulation efficiency α, namely the average particle diameter ratio before and after coagulation can be calculated by the formula 1:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
Preferably, the smoke box comprises: stainless steel shell, sealed fixing bolt, airtight jar body, variable speed fan, the annular air washes the pipeline, the control by temperature change probe, air inlet, jar body top cap, operating panel, reserve the detection mouth, the block terminal, inside and outside pressure balance device, the vacuum pump, airtight jar position is in stainless steel shell, variable speed fan, the annular air washes the pipeline and follows supreme airtight jar internal that is located in proper order down, air inlet, jar body top cap, operating panel all fixes on stainless steel shell's top, it is located jar body top cap to reserve the detection mouth, fix through sealed fixing bolt between jar body top cap and the stainless steel shell, the vacuum pump is located stainless steel shell and is located the side of airtight jar body.
Preferably, the X-ray microscope is Xradia 520Versa produced by Zeiss of Germany, can realize lossless three-dimensional structure imaging, and has the highest spatial resolution less than or equal to 0.7 mu m, or can be replaced by a microscope capable of realizing the same function.
Preferred example 3:
the preferred embodiment illustrates a method for measuring the coagulation efficiency of submicron particles on plant leaves by using an X-ray microscope, which comprises the following steps:
1. preparation of submicron particulate matter for laboratory simulation
In order to ensure that the particle size of submicron particles for laboratory simulation meets the test requirements, different saturated salt solutions are sequentially added into an aerosol generator, nitrogen is communicated to enable the particles to pass through a drying tube, and then distribution of different particle sizes of the particles is measured through a connected Grimm11-R particle size spectrometer, so that particles which meet the test requirements and have the particle size smaller than 1 mu m when emitted are obtained, wherein the particle size is more than 95 percent of the particle size, NaCl particles are selected in the example, and the emitted average particle size D is shown in figure 10It was 0.477 μm.
2. Sample collection and retention of particulate matter
2.1 Collection and processing of plant samples
According to the embodiment, common afforestation species camphor trees in Shanghai are selected as samples, fine-growing, sunny and small outer-layer branches are picked, the branches are immediately taken back, the atmospheric particles on the surface are washed away by flowing water, and finally the branches are washed by pure water, and then the branches are placed in a clean air environment to be naturally dried.
2.2 dust retention of plant samples
After the blades are dried, the blades are hung on a hook in the smoke box body and are covered with a box cover. Firstly, the environmental conditions are controlled at the temperature of 25 ℃ and the humidity of 50 percent required by research, the fan is turned on to stir the air in the box body, and the inner wall of the box body is flushed by pure nitrogen to ensure that PM in the box body1The concentration is reduced to 5 mu g/m3The following; blowing submicron particles into the box body by an aerosol generator filled with NaCl saturated solution, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to ensure that the submicron simulated particles are kept at 300-400 mu g/m3Within the range; the dust retention is stopped after 30 minutes,the blade is removed.
3. On-computer observation and data processing
3.1 scanning imaging with X-ray microscope
Randomly taking out three leaves, avoiding the midrib, the edge and the damaged part, carefully cutting off small leaves (with the width of about 2mm and the length of about 4mm) at a specific part by using a blade under a dissecting mirror; slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process; fixing the bottom of the blade on a special sample clamp of an X-ray microscope (model: Xradia 520Versa, Zeiss, a production company) by using special glue; setting relevant parameters of an X-ray microscope, namely voltage of 40-50 kV, power of 3-4W and objective lens multiplying power of 4-40X, and performing three-dimensional scanning imaging; after scanning, two-dimensional projection images of different sections with the voxel resolution of 0.7 mu m are obtained. And (3) combining professional three-dimensional view software and reconstruction software, performing three-dimensional reconstruction on the two-dimensional projection image to obtain a 3D image of the leaf sample, and generating about 1000 two-dimensional virtual slice images.
3.2 calculation of coagulation efficiency
The picture is imported into the matching software Dragonfly to obtain a 3D reconstructed image of the scanned part, as shown in fig. 2. Selecting the phase in a proper range in software to screen out the particles, checking the volume and the surface area to derive data, taking the NaCl particles as spheres approximately, calculating the particle size of the particles and the average particle size on the blade according to the volume and the surface area, and taking the average repeatedly for three times to obtain the average particle size D under the conditionC. In the examples, the average particle size (D) of particles on the leaf surface of camphor trees after 30 minutes of dust retention under the conditions of 25 ℃ of temperature and 50% of humidity is measuredC) 3.347 μm, passing through and the average particle diameter (D) at the time of emission0)0.477 μm contrast, it can be said that the particles are coagulated on the blade and the coagulation efficiency is
In addition, the same method is used for preparing the strip with the temperature of 40 ℃ and the humidity of 50%The average particle size (D) of the condensed blade surface particles is obtained by performing experiments under the conditionsC) 3.021 μm, the coagulation efficiency α is 6.33, and the comparison of the two efficiencies shows that the coagulation effect is better than 40 ℃ at 25 ℃.
In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
Those skilled in the art will appreciate that, in addition to implementing the systems, apparatus, and various modules thereof provided by the present invention in purely computer readable program code, the same procedures can be implemented entirely by logically programming method steps such that the systems, apparatus, and various modules thereof are provided in the form of logic gates, switches, application specific integrated circuits, programmable logic controllers, embedded microcontrollers and the like. Therefore, the system, the device and the modules thereof provided by the present invention can be considered as a hardware component, and the modules included in the system, the device and the modules thereof for implementing various programs can also be considered as structures in the hardware component; modules for performing various functions may also be considered to be both software programs for performing the methods and structures within hardware components.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. A method for measuring the coagulation efficiency of submicron particles on plant leaves is characterized by comprising the following steps:
preparing particles: preparing submicron-grade particles to simulate atmospheric particles, and marking the particle size as D0；
Simulating a dust retention step: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
and (3) coagulation efficiency obtaining step: taking out the dust-retention and adsorbed sample, cutting a small blade block with a preset size, wrapping the small blade block with a sealing film, fixing the bottom of the blade on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and performing quantitative analysis on the three-dimensional image by using image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
2. The method for measuring the coagulation efficiency of submicron particulate matters on plant leaves according to claim 1, wherein the particulate matter preparing step comprises:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0。
3. The method for measuring the coagulation efficiency of submicron particulate matters on plant leaves as claimed in claim 2, wherein the step of simulating dust retention is as follows:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blades are dried, the blades are hung on a hook in the smoke box body, and the smoke box cover is covered to control smokeThe environmental conditions in the box meet the requirements, the fan is turned on to stir the air in the box, and the inner wall of the box body is flushed by pure nitrogen to ensure that PM in the box body1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time, and taking out the blades.
4. The method for measuring the coagulation efficiency of submicron particulate matters on plant leaves according to claim 3, wherein the coagulation efficiency obtaining step comprises:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
5. The method of claim 4, wherein the smoke box comprises: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
the airtight jar of body is located the stainless steel shell, and variable speed fan, annular air wash the pipeline from supreme airtight jar of being located in proper order down internal, and air inlet, jar body top cap, operating panel all fix on the top of stainless steel shell, reserve and detect the mouth and be located a jar body top cap, fix through sealed fixing bolt between jar body top cap and the stainless steel shell, and the vacuum pump is located the stainless steel shell and is located the side of the airtight jar of body.
6. The method of claim 1, wherein the X-ray microscope comprises any one of the following:
xradia 520Versa, produced by Zeiss, germany, sub-micron resolution CT which can achieve the same functionality;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
7. A submicron particulate matter coagulation efficiency measurement system on plant leaf, characterized by comprising:
the particle preparation module comprises: preparation of submicron-sized particulate simulated atmospheric particulatesGranules with a particle size D0；
The simulation dust retention module: pretreating a plant leaf sample, putting the pretreated plant leaf sample into a smoke box connected with an aerosol generator, and keeping a certain submicron particulate matter concentration condition to enable the sample to carry out dust retention and adsorption for a preset time;
a coagulation efficiency acquisition module: taking out the dust-retention and adsorbed sample, cutting a small blade block with a preset size, wrapping the small blade block with a sealing film, fixing the bottom of the blade on a special sample clamp of an X-ray microscope, setting relevant parameters of the X-ray microscope, scanning and imaging, and performing quantitative analysis on the three-dimensional image by using image processing and three-dimensional reconstruction software to obtain the average particle size D of the particles on the sampleCAnd further can use the formula
The coagulation efficiency under this condition was calculated.
8. The system of claim 7, wherein the particulate preparation module:
the submicron-grade particles are saturated solution of salt, the proportion of particles with the particle size within a preset particle size range is more than a preset proportion when the aerosol is generated, and the average generated particle size is D0；
The simulation dust retention module:
picking fresh plant leaves meeting experimental requirements, immediately and repeatedly washing off atmospheric particles on the surface by using flowing water, finally washing once by using pure water, and then naturally airing the plant leaves in a ventilation environment of clean air;
after the blades are dried, the blades are hung on a hook in the smoke box body, a box cover is covered, the environmental conditions in the smoke box are controlled to meet the requirements, a fan is opened to stir the air in the box, the inner wall of the box body is washed by pure nitrogen, and PM in the box body is enabled to be1The concentration is reduced to be below the preset concentration;
blowing submicron simulation particles into the box body by using an aerosol generator, and monitoring the concentration of the particles in the box body in real time through a connected Grimm11-R particle size spectrometer to keep the submicron simulation particles at a high concentration level;
stopping dust retention after a preset time length, and taking out the blades;
the coagulation efficiency acquisition module:
carefully cutting a small blade block with a preset size at a specific position by using a blade under an anatomical lens;
slightly wrapping the cut small blade blocks with a sealing film, and compacting and fixing the edge of the sealing film along the edge of the blade by using a pair of tweezers to keep the moisture of the blade and prevent the blade from deforming in the scanning process;
fixing the bottom of the blade on a special sample clamp of an X-ray microscope by using special glue;
setting relevant parameters of an X-ray microscope, and performing three-dimensional scanning imaging;
the relevant parameters include: voltage, power and objective magnification;
importing the pictures into image processing and three-dimensional reconstruction software, screening out particles contained in the sample, and exporting the volume Vi of the particles;
the coagulation efficiency α, i.e., the average particle diameter ratio before and after coagulation, is calculated as follows:
wherein the content of the first and second substances,
α denotes coagulation efficiency;
D0represents the average particle size at which the particulate matter is emitted;
DCthe average particle size of the condensed leaf surface particles is expressed, the particles can be approximated to spheres, and the average particle size is calculated by a sphere volume formula;
n represents the total number of the screened particles.
9. The system of claim 8, wherein the smoke box comprises: the device comprises a stainless steel shell, a sealing fixing bolt, a sealed tank body, a variable speed fan, an annular air flushing pipeline, a temperature control probe, an air inlet, a tank body top cover, an operation panel, a reserved detection port, a distribution box, an internal and external pressure balancing device and a vacuum pump;
the sealed tank body is positioned in the stainless steel shell, the variable speed fan and the annular air flushing pipeline are sequentially positioned in the sealed tank body from bottom to top, the air inlet, the tank body top cover and the operation panel are all fixed on the top end of the stainless steel shell, the reserved detection port is positioned on the tank body top cover, the tank body top cover and the stainless steel shell are fixed through a sealing fixing bolt, and the vacuum pump is positioned in the stainless steel shell and positioned on the side face of the sealed tank body;
the X-ray microscope includes any one of:
xradia 520Versa, produced by Zeiss, Germany, can realize the same functional sub-micron resolution CT;
the Xradia 520Versa produced by German Zeiss can realize lossless three-dimensional structure imaging, the highest spatial resolution is less than or equal to 0.7 mu m, and the voltage adjustable range is 30-160 kV.
10. A computer-readable storage medium storing a computer program, wherein the computer program when executed by a processor implements the steps of the method for determining the coagulation efficiency of submicron particulate matter on plant leaves according to any one of claims 1 to 6.
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